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Methyldiethoxyphosphine, also known as Dimethyl methylphosphonate, is a phosphonite reagent derived from the chemical synthesis of various organic compounds. It possesses unique chemical properties that make it a versatile building block in the pharmaceutical and chemical industries. Its phosphonite group allows for the formation of phosphinic acid derivatives and its chiral nature makes it a valuable intermediate in the synthesis of complex molecules.

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  • 15715-41-0 Structure
  • Basic information

    1. Product Name: Methyldiethoxyphosphine
    2. Synonyms: DIETHOXYMETHYLPHOSPHINE;DIETHYL METHYLPHOSPHONITE;METHYLDIETHOXYPHOSPHINE;O,O-diethyl methylphosphonite;Methyldiethoxyphosphine,99%;METHYL-PHOSPHONOUS ACI DIETHYL ESTER;Methylphosphonous acid diethyl ester;diethoxy(methyl)phosphane
    3. CAS NO:15715-41-0
    4. Molecular Formula: C5H13O2P
    5. Molecular Weight: 136.13
    6. EINECS: 239-805-9
    7. Product Categories: Phosphorus compounds
    8. Mol File: 15715-41-0.mol
  • Chemical Properties

    1. Melting Point: N/A
    2. Boiling Point: 124.497 °C at 760 mmHg
    3. Flash Point: 38°C
    4. Appearance: /Liquid
    5. Density: 0,9 g/cm3
    6. Vapor Pressure: 15.4mmHg at 25°C
    7. Refractive Index: 1.4168
    8. Storage Temp.: 2-8°C
    9. Solubility: N/A
    10. Water Solubility: It slowly hydrolyses in water.
    11. Sensitive: Air & Moisture Sensitive
    12. CAS DataBase Reference: Methyldiethoxyphosphine(CAS DataBase Reference)
    13. NIST Chemistry Reference: Methyldiethoxyphosphine(15715-41-0)
    14. EPA Substance Registry System: Methyldiethoxyphosphine(15715-41-0)
  • Safety Data

    1. Hazard Codes: Xn
    2. Statements: 10-36/37/38-22
    3. Safety Statements: 16-26-36/37/39
    4. RIDADR: 1993
    5. WGK Germany: 3
    6. RTECS:
    7. TSCA: Yes
    8. HazardClass: 6.1
    9. PackingGroup: II
    10. Hazardous Substances Data: 15715-41-0(Hazardous Substances Data)

15715-41-0 Usage

Uses

Used in Pharmaceutical Industry:
Methyldiethoxyphosphine is used as a key intermediate for the synthesis of various pharmaceutical compounds. Its chiral nature and reactivity make it a promising candidate for the development of new drugs and therapeutic agents.
Used in Chemical Synthesis:
Methyldiethoxyphosphine is used as a cyclization reagent in the preparation of 2-substituted penems, a class of β-lactam antibiotics. Its ability to form phosphinic acid derivatives via the Arbuzov reaction makes it a valuable building block in the synthesis of complex organic molecules.
Used in Research and Development:
Methyldiethoxyphosphine is used as a chiral intermediate in the development of new chemical processes and methodologies. Its unique properties and reactivity make it an important tool for researchers in the field of organic chemistry and drug discovery.

Check Digit Verification of cas no

The CAS Registry Mumber 15715-41-0 includes 8 digits separated into 3 groups by hyphens. The first part of the number,starting from the left, has 5 digits, 1,5,7,1 and 5 respectively; the second part has 2 digits, 4 and 1 respectively.
Calculate Digit Verification of CAS Registry Number 15715-41:
(7*1)+(6*5)+(5*7)+(4*1)+(3*5)+(2*4)+(1*1)=100
100 % 10 = 0
So 15715-41-0 is a valid CAS Registry Number.
InChI:InChI=1/C5H13O2P/c1-4-6-8(3)7-5-2/h4-5H2,1-3H3

15715-41-0 Well-known Company Product Price

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  • Detail
  • Alfa Aesar

  • (30357)  Diethyl methylphosphonite   

  • 15715-41-0

  • 0.5g

  • 301.0CNY

  • Detail
  • Alfa Aesar

  • (30357)  Diethyl methylphosphonite   

  • 15715-41-0

  • 0.2g

  • 337.0CNY

  • Detail
  • Alfa Aesar

  • (30357)  Diethyl methylphosphonite   

  • 15715-41-0

  • 2g

  • 600.0CNY

  • Detail
  • Alfa Aesar

  • (30357)  Diethyl methylphosphonite   

  • 15715-41-0

  • 10g

  • 2134.0CNY

  • Detail
  • Aldrich

  • (762334)  Diethyl methylphosphonite  97%

  • 15715-41-0

  • 762334-1G

  • 338.13CNY

  • Detail
  • Aldrich

  • (762334)  Diethyl methylphosphonite  97%

  • 15715-41-0

  • 762334-5G

  • 1,235.52CNY

  • Detail
  • Aldrich

  • (762334)  Diethyl methylphosphonite  97%

  • 15715-41-0

  • 762334-10G

  • 2,027.61CNY

  • Detail

15715-41-0SDS

SAFETY DATA SHEETS

According to Globally Harmonized System of Classification and Labelling of Chemicals (GHS) - Sixth revised edition

Version: 1.0

Creation Date: Aug 14, 2017

Revision Date: Aug 14, 2017

1.Identification

1.1 GHS Product identifier

Product name Methyldiethoxyphosphine

1.2 Other means of identification

Product number -
Other names Diethoxymethylphosphine

1.3 Recommended use of the chemical and restrictions on use

Identified uses For industry use only.
Uses advised against no data available

1.4 Supplier's details

1.5 Emergency phone number

Emergency phone number -
Service hours Monday to Friday, 9am-5pm (Standard time zone: UTC/GMT +8 hours).

More Details:15715-41-0 SDS

15715-41-0Synthetic route

ethanol
64-17-5

ethanol

methyldichlorophosphane
676-83-5

methyldichlorophosphane

methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

Conditions
ConditionsYield
With triethylamine In Petroleum ether at 25 - 60℃; for 1.5h; Time; Flow reactor; Large scale;98%
Stage #1: ethanol With calcium oxide In 1,3,5-trimethyl-benzene for 2h; Reflux;
Stage #2: methyldichlorophosphane In 1,3,5-trimethyl-benzene at 0 - 30℃; for 4h; Temperature; Solvent; Inert atmosphere;
96.7%
at 10 - 120℃; for 0.0833333h; Temperature; Inert atmosphere;96%
diethyl phosphorylchloridite
589-57-1

diethyl phosphorylchloridite

methylmagnesium chloride
676-58-4

methylmagnesium chloride

methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

Conditions
ConditionsYield
Stage #1: diethyl phosphorylchloridite; methylmagnesium chloride In tetrahydrofuran at -10 - 0℃; for 2h; Inert atmosphere;
Stage #2: With dibutyl ether; benzylamine In tetrahydrofuran at -5℃; for 10h; Reagent/catalyst; Temperature;
89.3%
In tetrahydrofuran at 0℃; for 2.5h; Temperature;
In tetrahydrofuran at -10 - -5℃; Inert atmosphere;10.15 g
diethyl phosphorylchloridite
589-57-1

diethyl phosphorylchloridite

methyl magnesium iodide
917-64-6

methyl magnesium iodide

methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

Conditions
ConditionsYield
In diethyl ether60%
diethyl peroxide
628-37-5

diethyl peroxide

1,3,4-trimethyl-Δ3-phospholene
14410-05-0

1,3,4-trimethyl-Δ3-phospholene

A

methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

B

Diethyl methylphosphonate
683-08-9

Diethyl methylphosphonate

C

tetraethoxy-methyl-λ5-phosphane
34736-63-5

tetraethoxy-methyl-λ5-phosphane

D

1,3,4-trimethyl-Δ3-phospholene oxide
15450-80-3

1,3,4-trimethyl-Δ3-phospholene oxide

E

1,3,4-trimethyl-2,3-dihydro-1H-phosphole 1-oxide
15450-82-5

1,3,4-trimethyl-2,3-dihydro-1H-phosphole 1-oxide

Conditions
ConditionsYield
In [D3]acetonitrile for 1.91667h; Rate constant; Product distribution; further reaction times;A 10 % Spectr.
B 6 % Spectr.
C 15 % Spectr.
D 7 % Spectr.
E n/a
diethyl phosphorylchloridite
589-57-1

diethyl phosphorylchloridite

methylmagnesium bromide
75-16-1

methylmagnesium bromide

methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

Conditions
ConditionsYield
In diethyl ether at -12 - 0℃; for 16h;30.4 g
In diethyl ether -20 deg C then r.t., 1 h;
methylmagnesium bromide
75-16-1

methylmagnesium bromide

triethyl phosphite
122-52-1

triethyl phosphite

methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

diethyl phosphorylchloridite
589-57-1

diethyl phosphorylchloridite

methylene chloride
74-87-3

methylene chloride

methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

Conditions
ConditionsYield
Stage #1: methylene chloride With magnesium In tetrahydrofuran; toluene for 2h;
Stage #2: diethyl phosphorylchloridite In tetrahydrofuran; toluene at 15 - 30℃; for 6h; Solvent; Temperature;
ethanol
64-17-5

ethanol

trichloro-methyl-phosphonium; compound of chloride with aluminium chloride

trichloro-methyl-phosphonium; compound of chloride with aluminium chloride

methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

Conditions
ConditionsYield
With aluminium at -10 - 150℃; for 2h; Temperature;71.62 g
methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

ethyl methylphosphinate
16391-07-4

ethyl methylphosphinate

Conditions
ConditionsYield
With water at 22℃; for 17h;100%
With water at 5 - 20℃; for 18h;
In water at 0 - 22℃; for 17h;
With water; hexadecyltributylammonium chloride; sodium chloride at -5 - 0℃; Inert atmosphere;8.8 g
With water at 20℃; for 18h; Inert atmosphere;
methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

1-Chloromethylnaphthalene
86-52-2

1-Chloromethylnaphthalene

C14H17O2P
936366-26-6

C14H17O2P

Conditions
ConditionsYield
for 2.5h; Heating;100%
methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

butan-1-ol
71-36-3

butan-1-ol

butyl methylphosphinate
6172-80-1

butyl methylphosphinate

Conditions
ConditionsYield
Stage #1: methyldiethoxyphosphine; butan-1-ol In water; toluene at 45 - 50℃; for 5h; Inert atmosphere;
Stage #2: With tetrabutoxytitanium In water; toluene Reflux;
98.26%
With Amberlyst 15 In water; toluene at 50 - 140℃; Inert atmosphere;97.9%
ethyl 6-chloro-6-oxohexanoate
1071-71-2

ethyl 6-chloro-6-oxohexanoate

methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

5-Ethoxy-adipyl-P-methyl-phosphinsaeure-O-ethylester
115693-04-4

5-Ethoxy-adipyl-P-methyl-phosphinsaeure-O-ethylester

Conditions
ConditionsYield
at 30℃;98%
methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

[(E)-(R)-4-[(1R,2R,3S,5R)-2-((Z)-6-Bromo-hex-2-enyl)-3,5-bis-(tert-butyl-dimethyl-silanyloxy)-cyclopentyl]-2-(tert-butyl-dimethyl-silanyloxy)-but-3-enyloxy]-benzene
380153-45-7

[(E)-(R)-4-[(1R,2R,3S,5R)-2-((Z)-6-Bromo-hex-2-enyl)-3,5-bis-(tert-butyl-dimethyl-silanyloxy)-cyclopentyl]-2-(tert-butyl-dimethyl-silanyloxy)-but-3-enyloxy]-benzene

(6-{3,5-bis(tert-butyldimethylsilanoylxy)-2-[3-(tert-cutyldimethylsilanoylxy)-4-phenoxybut-1-enyl]cyclopentyl}-hex-4-enyl)methylphosphinic acid ethyl ester
380153-32-2

(6-{3,5-bis(tert-butyldimethylsilanoylxy)-2-[3-(tert-cutyldimethylsilanoylxy)-4-phenoxybut-1-enyl]cyclopentyl}-hex-4-enyl)methylphosphinic acid ethyl ester

Conditions
ConditionsYield
In toluene at 145℃; for 22h; Arbuzov reaction;98%
methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

4-bromomethylphenylboronic acid pinacol ester
138500-85-3

4-bromomethylphenylboronic acid pinacol ester

ethyl methyl(4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzyl)phosphinate
1273492-75-3

ethyl methyl(4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzyl)phosphinate

Conditions
ConditionsYield
In 1,4-dioxane at 100℃; for 1h; Inert atmosphere;98%
methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

(S)-tert-butyl 3-((4-(7-bromo-1H-indol-3-yl)-5-(trifluoromethyl)pyrimidin-2-yl)amino)piperidine-1-carboxylate

(S)-tert-butyl 3-((4-(7-bromo-1H-indol-3-yl)-5-(trifluoromethyl)pyrimidin-2-yl)amino)piperidine-1-carboxylate

(S)-tert-butyl 3-((4-(7-(ethoxy(methyl)phosphoryl)-1H-indol-3-yl)-5-(trifluoromethyl)pyrimidin-2-yl)amino)piperidine-1-carboxylate

(S)-tert-butyl 3-((4-(7-(ethoxy(methyl)phosphoryl)-1H-indol-3-yl)-5-(trifluoromethyl)pyrimidin-2-yl)amino)piperidine-1-carboxylate

Conditions
ConditionsYield
With dichloro(1,1'-bis(diphenylphosphanyl)ferrocene)palladium(II)*CH2Cl2; triethylamine In N,N-dimethyl-formamide at 130℃; for 0.0833333h; Sealed tube; Microwave irradiation;98%
methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

tert-Butyl acrylate
1663-39-4

tert-Butyl acrylate

C10H21O4P

C10H21O4P

Conditions
ConditionsYield
With acetic acid at 70 - 75℃; for 4h; Inert atmosphere;97.6%
methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

acrylic acid methyl ester
292638-85-8

acrylic acid methyl ester

methyl 3-(methylethoxyphosphoryl)propionate

methyl 3-(methylethoxyphosphoryl)propionate

Conditions
ConditionsYield
With acetic acid at 5 - 20℃; for 2h;96.3%
methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

1-bromomethyl-3-methoxy-4-nitrobenzene
23145-65-5

1-bromomethyl-3-methoxy-4-nitrobenzene

(3-methoxy-4-nitrobenzyl)-methyl phosphonic acid ethyl ester
1257996-50-1

(3-methoxy-4-nitrobenzyl)-methyl phosphonic acid ethyl ester

Conditions
ConditionsYield
In toluene for 16h; Reflux;96%
methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

ethyl acrylate
140-88-5

ethyl acrylate

ethyl 3-(ethoxymethylphosphinyl)propionate
15090-27-4

ethyl 3-(ethoxymethylphosphinyl)propionate

Conditions
ConditionsYield
In ethanol at 5℃; for 2h;95.8%
With acetic acid at 5 - 25℃; for 2.5h; Inert atmosphere;95%
pentan-1-ol
71-41-0

pentan-1-ol

methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

pentyl hydrogen methylphosphonite
87025-52-3

pentyl hydrogen methylphosphonite

Conditions
ConditionsYield
With sulfuric acid In water at 50℃; Reflux;95.8%
methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

ethyl 2-iodobenzoate
1829-28-3

ethyl 2-iodobenzoate

o-ethoxycarbonylphenyl-methylphosphinic acid ethyl ester
57020-81-2

o-ethoxycarbonylphenyl-methylphosphinic acid ethyl ester

Conditions
ConditionsYield
With nickel dichloride at 170℃;95%
methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

C26H33BrO3Si
1215320-42-5

C26H33BrO3Si

C29H41O5PSi
1215320-44-7

C29H41O5PSi

Conditions
ConditionsYield
at 110℃; for 17h; Michaelis-Arbuzov reaction;95%
ethanol
64-17-5

ethanol

methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

acetic anhydride
108-24-7

acetic anhydride

acrolein
107-02-8

acrolein

1-acetoxy-1-ethoxy-3-(ethoxy(methyl)phosphinyl)propane

1-acetoxy-1-ethoxy-3-(ethoxy(methyl)phosphinyl)propane

Conditions
ConditionsYield
at 25 - 30℃; for 2.33333h; Inert atmosphere;95%
methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

Bromoacetaldehyde diethyl acetal
2032-35-1

Bromoacetaldehyde diethyl acetal

2-(ethoxy(methylphosphoryl))acetaldehyde diethyl acetal

2-(ethoxy(methylphosphoryl))acetaldehyde diethyl acetal

Conditions
ConditionsYield
In ethanol at 80 - 100℃; for 24h; Solvent;95%
In toluene at 110℃; for 4h; Arbuzov Reaction;91%
methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

trimethylammonium methylformamide

trimethylammonium methylformamide

O-ethyl-formyl-aminomethyl-methylphosphinate

O-ethyl-formyl-aminomethyl-methylphosphinate

Conditions
ConditionsYield
94%
methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

1-bromo-5,9-bis[N-(2-mesitylene)sulfonyl]-12-{N-ethyl-N-[(2-mesitylene)sulfonyl]}amino-5,9-diazadodecane

1-bromo-5,9-bis[N-(2-mesitylene)sulfonyl]-12-{N-ethyl-N-[(2-mesitylene)sulfonyl]}amino-5,9-diazadodecane

{4-[{3-[{3-[Ethyl-(2,4,6-trimethyl-benzenesulfonyl)-amino]-propyl}-(2,4,6-trimethyl-benzenesulfonyl)-amino]-propyl}-(2,4,6-trimethyl-benzenesulfonyl)-amino]-butyl}-methyl-phosphinic acid ethyl ester

{4-[{3-[{3-[Ethyl-(2,4,6-trimethyl-benzenesulfonyl)-amino]-propyl}-(2,4,6-trimethyl-benzenesulfonyl)-amino]-propyl}-(2,4,6-trimethyl-benzenesulfonyl)-amino]-butyl}-methyl-phosphinic acid ethyl ester

Conditions
ConditionsYield
at 125℃; for 3h;94%
2-bromomethyl-1,3-dioxolane
4360-63-8

2-bromomethyl-1,3-dioxolane

methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

2-(ethoxy(methylphosphoryl))acetaldehyde ethylene acetal

2-(ethoxy(methylphosphoryl))acetaldehyde ethylene acetal

Conditions
ConditionsYield
In toluene at 110℃; for 5h; Inert atmosphere;93.8%
at 120℃; for 2h; Arbuzov Reaction;82.6%
4-acetoxy azetidinone
28562-53-0

4-acetoxy azetidinone

methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

O-ethyl(4-oxoazetidin-2-yl)methylphosphinate
84673-24-5

O-ethyl(4-oxoazetidin-2-yl)methylphosphinate

Conditions
ConditionsYield
at 60℃; for 1h;93%
at 60℃; for 1h;89%
methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

C9H16ClNO4

C9H16ClNO4

C12H24NO6P

C12H24NO6P

Conditions
ConditionsYield
With lanthanum(III) chloride at 140℃; for 10h; Reagent/catalyst; Temperature; Inert atmosphere;91.3%
1,1-dimethylethyl [4-(bromomethyl)-1,3-thiazol-2-yl]carbamate
1001419-35-7

1,1-dimethylethyl [4-(bromomethyl)-1,3-thiazol-2-yl]carbamate

methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

C12H21N2O4PS
1001419-75-5

C12H21N2O4PS

Conditions
ConditionsYield
In tetrahydrofuran at 75℃; for 16h;91%
methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

C11H20ClNO4

C11H20ClNO4

C14H28NO6P

C14H28NO6P

Conditions
ConditionsYield
With tetrabutylammomium bromide; magnesium bromide In water at 140℃; for 15h; Temperature; Solvent; Reagent/catalyst;90.2%
methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

4-bromo-2-phthalimidobutyric acid methyl ester
122690-13-5

4-bromo-2-phthalimidobutyric acid methyl ester

METHYL DL-2-(1,3-DIHYDRO-1,3-DIOXO-2H-ISOINDOL-2-YL)-4-(ETHOXYMETHYLPHOSPHINYL)BUTANOATE
109541-73-3

METHYL DL-2-(1,3-DIHYDRO-1,3-DIOXO-2H-ISOINDOL-2-YL)-4-(ETHOXYMETHYLPHOSPHINYL)BUTANOATE

Conditions
ConditionsYield
In toluene at 100℃;90%
methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

6-Bromohexanoic Acid Phenylamide
7661-21-4

6-Bromohexanoic Acid Phenylamide

methyl-(5-phenylcarbamoyl-pentyl)-phosphinic acid ethyl ester
606092-26-6

methyl-(5-phenylcarbamoyl-pentyl)-phosphinic acid ethyl ester

Conditions
ConditionsYield
at 120℃; for 10h;89%
at 120℃; for 10h; Arbuzov reaction;200 mg
methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

ethyl 2-oxo-3-butenoate
134745-23-6

ethyl 2-oxo-3-butenoate

ethyl 4-(methylethoxyphosphoryl)-2-oxobutanoate

ethyl 4-(methylethoxyphosphoryl)-2-oxobutanoate

Conditions
ConditionsYield
at 5℃; for 8h; Inert atmosphere;87.8%
methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

Methyl-3-oxo-pentenoat
108736-44-3

Methyl-3-oxo-pentenoat

methyl 4-(methylethoxyphosphoryl)-2-oxobutanoate

methyl 4-(methylethoxyphosphoryl)-2-oxobutanoate

Conditions
ConditionsYield
In tetrahydrofuran at 5℃; for 6h; Inert atmosphere;87.1%
methyldiethoxyphosphine
15715-41-0

methyldiethoxyphosphine

2-decarboxy-2-iodoprostaglandin F2α triacetate
252858-13-2

2-decarboxy-2-iodoprostaglandin F2α triacetate

2-decarboxy-2-(O-ethyl-P-methylphosphinico)prostaglandin F2α triacetate
380153-41-3

2-decarboxy-2-(O-ethyl-P-methylphosphinico)prostaglandin F2α triacetate

Conditions
ConditionsYield
In toluene at 100℃; for 6h; Arbuzov reaction;86%

15715-41-0Relevant articles and documents

Synthesis method and synthesis device of diethyl methylphosphite

-

Paragraph 0071-0118, (2020/09/09)

The invention relates to a synthesis method and a synthesis device of diethyl methylphosphite. The synthesis method comprises the following steps: (1) mixing methyl phosphine dichloride, absolute ethyl alcohol and a solvent to carry out a synthesis reaction; (2) carrying out reduced pressure deacidification treatment on the reaction solution obtained in the step (1); and (3) separating and purifying the deacidified reaction solution obtained in the step (2) to obtain diethyl methylphosphite. According to the synthesis method, an acid-binding agent is not needed, hydrogen chloride gas generatedby the synthesis reaction can be discharged through reduced-pressure deacidification treatment, the generation of solid waste residues containing acid-binding agent hydrochloride is avoided, the separation and treatment of the solid waste residues are reduced, and the dosage of ethanol is reduced by adding a solvent, so that the ethanol does not need to play a role as a solvent, the energy consumption is reduced, the resources are saved, the process is high in yield, simple to operate and environment-friendly, and the atom economy is good.

Purification method of dialkyl methylphosphite

-

Paragraph 0041-0043; 0047-0052; 0059-0067; 0074-0083, (2020/12/15)

The invention relates to the technical field of compound purification, and particularly provides a purification method of dialkyl methylphosphite. The purification method comprises the following steps: adding a weak polar solvent into a reaction solution containing dialkyl methylphosphite, magnesium chloride and an ether solvent, conducting cooling to -10 DEG C to 40 DEG C, adding a nitrogen-containing organic alkali compound, carrying out a heat preservation reaction, and conducting filtering to obtain magnesium chloride and a filtrate; and rectifying the filtrate to obtain a dialkyl methylphosphite product. According to the purification method provided by the invention, the purity and the yield of the dialkyl methylphosphite are improved, the obtained magnesium chloride does not containcrystal water, the nitrogen content in the magnesium chloride is 0.01-0.5%, and the purity of the anhydrous magnesium chloride can reach 97% or above; and the purity of the obtained dialkyl methylphosphite product can reach 97% or above, and the yield can reach 85% or above. The method has the advantages of simple process, no need of special equipment, mild reaction conditions and no need of high-temperature distillation or low-temperature brine treatment process, and is suitable for large-scale industrial production.

A method for preparing methyl asia phosphine acid diethyl ester (by machine translation)

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Paragraph 0028-0032, (2019/07/06)

The invention discloses a method for preparing methyl asia phosphine acid diethyl ester, aims to solve the problems in the existing method, when using ammonia gas as acid, pH value of the reaction solution in the need to control the 7.0 - 8.5 between, accurate control of the pH value is very difficult, and is lower than the pH value, will produce a large number of methyl inferior phosphine acid ethyl ester by-product, the use of the organic amine do capture, there is caused a large toxicity, high price, the recovery process is tedious, the recovery rate is low. The present invention relates to methyl-phosphine, ethanol and calcium oxide as the main raw material, process for preparing methyl asia phosphine acid diethyl ester is obtained, which is a low-cost, is suitable for the industrial production of methyl asia phosphine acid diethyl ester preparation method. The invention in the preparation of the methyl asia phosphine acid diethyl ester, for the first time the adoption of the calcium oxide to replace the ammonia or organic amine as capture, effectively reduces the production cost, and the calcium oxide is non-toxic, is friendly to the environment, and has a good economic value and social value. (by machine translation)

A method for preparing methyl asia phosphine acid diethyl ester

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Paragraph 0036; 0037; 0038; 0039-0045, (2019/05/04)

The invention provides a method for synthesizing diethyl methyl-phosphonite. The method comprises technological steps as follows: firstly, a ternary complex is prepared from phosphorus trichloride, aluminium trichloride and chloromethane as raw materials, the ternary complex is reduced by powdered aluminium and reacts with absolute ethyl alcohol, a crude diethyl methyl-phosphonite product is obtained and subjected to reduced-pressure distillation, and a pure product is obtained. According to the method, diethyl methyl-phosphonite is directly prepared from the ternary complex, an intermediate methyl phosphonic dichloride is not needed, and dangerous level of industrial production is reduced; compared with a traditional technology for preparing diethyl methyl-phosphonite from the intermediate methyl phosphonic dichloride, ethyl alcohol and sodium chloride through a reaction, the reaction conditions are milder, waste residue rate is obviously reduced, and yield is as high as 85%.

Methyl asia phosphine acid ester compound synthesis and purification method

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Paragraph 0061; 0062; 0063, (2018/02/04)

The invention relates to a synthesis and purification method of methyl phosphinate compounds. The method concretely comprises the following steps: adding brine to a solution containing a methyldialkyl phosphinate and magnesium chloride mixture in an inert solvent at a low temperature, and separating to obtain methylalkyl phosphinate or methyldialkyl phosphinate. The method solves the post-treatment and purification difficulties of a Grignard reagent method, and has the advantages of industrial production, effective reduction of the generation of methyl phosphonous acid, mild process conditions, and excellent reaction yield and product quality.

Preparation method of dialkyl methylphosphonite

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Paragraph 0047-0054; 0064-0077, (2018/02/04)

The invention relates to a preparation method of dialkyl methylphosphonite. tertiary amine with pKa greater than 10 is adopted as the acid binding agent, methyl phosphonic dichloride and alcohol react in a solvent, and the mole ratio of the methyl phosphonic dichloride, alcohol and tertiary amine is 1:2.0-2.4:2.0-2.4, the produced tertiary amine hydrochloride is neutralized with a caustic soda aqueous solution, and the solvent and tertiary amine obtained by evaporation is recycled and reused. The alkyl of the dialkyl methylphosphonite is straight chain and side chain alkane or alkene of aliphatic C1-C4, the alcohol refers to methanol, ethanol, propanol, isopropanol, allyl alcohol, n-butanol, isobutanol and the like, the tertiary amine refers to tertiary fatty amine, and also refers to fatty group and aromatic mixed tertiary amine, at the same time, the pKa of the tertiary amine is required to be greater than 10, and the tertiary amine can include triethylamine, tripropylamine and tributylamine.

A kind of preparation method for treating keratoconjunctival and wherein the intermediate preparation method

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Paragraph 0117; 0118, (2017/03/08)

The invention relates to the technical field of pesticides and particularly relates to a method for preparing glufosinate-ammonium and a preparation method for an intermediate thereof. The method is characterized by comprising the following steps of: taking phosphorus trichloride and phosphite ester as raw materials, preparing chlorophosphite ester under the catalysis of the mixture of triethylamine, N,N-dimethylformamide or pyridine and hexamethylphosphoramide, preparing methylmagnesium chloride from chloromethane and magnesium metal, preparing methyl phosphite ester by reacting the chlorophosphite ester with methylmagnesium chloride, carrying out an addition reaction on the methyl phosphite ester and acrolein, carrying out a Strecker reaction on the product of the addition reaction, sodium cyanide, ammonium chloride and ammonia water under the catalysis of montmorillonite-supported lewis acid, and carrying out hydrolyzing and purifying after finishing the Strecker reaction, so as to obtain the high-purity glufosinate-ammonium. The method provided by the invention has the advantages that side reactions are few, products are high in purity and easy to separate, and catalysts and solvents are easy to obtain, regenerate and recycle; and the production cost is lowered, and the method is accordant with the trend of green chemical industry and is suitable for industrial production.

Synthetic method of methyl phosphite and glufosinate-ammonium

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Paragraph 0033; 0052, (2016/11/07)

The invention discloses a synthetic method of methyl phosphite and glufosinate-ammonium. The method comprises the steps: with phosphorus pentasulfide as a starting material, then carrying out vulcanization reaction, chlorination reaction, water washing and distillation purification, then carrying out catalytic hydrogenation to obtain chloride phosphite (III), and next carrying out Grignard reaction to obtain methyl phosphite (IV), wherein R is C1-C4 alkyl. The method comprises the steps: with phosphorus pentasulfide as the starting material, then carrying out vulcanization reaction, chlorination reaction, water washing and distillation purification, then carrying out catalytic hydrogenation to obtain chloride phosphite, next carrying out Grignard reaction to synthesize methyl phosphite (IV), and thus obtaining the final product glufosinate-ammonium through a Strecker route of the prior art. The synthetic yield is increased, methyl phosphorus dichloride and other unstable corrosive intermediates cannot be produced, the discharge of three-waste substances is reduced, and environment-friendly costs and pressure are reduced.

Direct α-chlorination of O,O-dialkyl chalcogenophosphonates with phosphorus oxychloride

Mons, Stéphane,Sabourault, Nicolas,Klein, Emmanuel,Mioskowski, Charles,Lebeau, Luc

, p. 7547 - 7549 (2007/10/03)

α-Chlorination of phosphonates, and O,O-dialkyl thio- and selenophosphonates involving the direct reaction of their lithiated anion with phosphorus oxychloride is described. The reaction gives good results where previously known methods fail. The role of the chalcogen atom, and the influence of the nature of the alkyl chain with respect to the reactivity are discussed.

Synthesis, NMR, relaxometry and circularly polarised luminescence studies of macrocyclic monoamidetris(phosphinate) complexes bearing a remote chiral centre

Aime, Silvio,Botta, Mauro,Dickins, Rachel S.,Maupin, Christine L.,Parker, David,Riehl, James P.,Williams, J. A. Gareth

, p. 881 - 892 (2007/10/03)

Lanthanide complexes of macrocyclic monoamidetris(phosphinate) ligands are partially hydrated in aqueous solution. Introduction of a chiral centre into the amide group leads to the formation of only two non-interconverting complex diastereoisomers (2:1 for α-phenylethyl and 4:1 for α-1-naphthylethyl). Proton, 31P NMR and circularly polarised luminescence studies indicated that the configuration at the chiral carbon centre determines the helicity of the layout of the pendent arms and the macrocyclic ring conformation, with an RRR or SSS configuration preferred at the phosphorus centres.

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