cas 763-69-9, Ethyl-3-ethoxypropanoate | Articles data

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Synthesis method of ethyl 3-ethoxypropionate
The invention relates to a synthesis method of ethyl 3-ethoxypropionate, which comprises the following steps of carrying out addition reaction on absolute ethyl alcohol and ethyl acrylate in the presence of a catalyst which is a micromolecular tertiary amine catalyst, after the reaction is finished, removing excessive absolute ethyl alcohol, unreacted ethyl acrylate and the catalyst through rectification, collecting ethyl 3-ethoxypropionate with the purity being greater than 99.8% as a product, and recycling the collected excessive absolute ethyl alcohol, unreacted ethyl acrylate and the catalyst in the next reaction. The synthesis method has the advantages of simple synthesis, mild conditions, no need of acid neutralization, few side reactions, no three wastes, high conversion rate, long-term use of the catalyst, repeated cyclic utilization, no damage, simplified separation process, good product quality, easy obtainment of 99.8% or above of purity, promotion of large-scale production,and facilitation of large-scale application to the photoelectric industry.
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Paragraph 0042-0068

(2021/03/13)

One-pot production of diethyl maleate via catalytic conversion of raw lignocellulosic biomass
The conversion of lignocellulose into a value-added chemical with high selectivity is of great significance but is a big challenge due to the structural diversities of biomass components. Here, we have reported an efficient approach for the one-step conversion of raw lignocellulose into diethyl maleate by the polyoxometalate ionic liquid [BSmim]CuPW12O40 in ethanol under mild conditions. The results reveal that all of the fractions in biomass, i.e., cellulose, lignin and hemicellulose, were simultaneously converted into diethyl maleate (DEM), achieving a 329.6 mg g-1 yield and 70.3% selectivity from corn stalk. Importantly, the performance of the ionic liquid catalyst [BSmim]CuPW12O40 was nearly twice that of CuHPW12O40, which can be attributed to the lower incorporation of the Cu2+ site in [BSmim]CuPW12O40. Hence, this process opens a promising route for producing bio-based bulk chemicals from raw lignocellulose without any pretreatment.
Cai, Zhenping,Chen, Rujia,Jiang, Lilong,Li, Fukun,Li, Xuehui,Long, Jinxing,Zhang, Hao
supporting information
p. 10116 - 10122
(2021/12/24)

Method for producing Alkyl 3-Alkoxypropionate Using Continuous Type Process
The invention relates to a process for preparing alkyl 3 - alkoxypropionates. More particularly, it relates to a continuous process for preparing ethyl 3 - ethoxypropionate. A method for preparing an alkyl 3 - alkoxypropionate for a semiconductor is provided to produce alkyl 3 - alkoxypropionate for a semiconductor on a large scale using a continuous reaction, and to prepare an alkyl 3 - 3 - alkoxypropionate for a semiconductor in a large scale production process using a continuous method.
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Paragraph 0077-0087

(2021/01/09)

Method for producing Ethyl 3-Ethoxypropionate
The present invention relates to a method for manufacturing ethyl 3-ethoxypropionate (EEP), comprising a step of synthesizing EEP with an ethyl acrylate monomer and ethanol in the presence of a catalyst, and then efficiently regenerating unreacted ethanol and the ethyl acrylate monomer from a reaction product obtained by removing a salt. It is possible to increase economic feasibility of EEP by efficiently regenerating and reusing, especially, ethanol among reaction products.COPYRIGHT KIPO 2019
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Paragraph 0021

(2019/09/11)

Method for Producing Alkyl 3-Alkoxy Propionate
The present invention relates to a method for manufacturing alkyl 3-alkoxypropionate. The present invention relates to a method for manufacturing alkoxypropionate which can increase the conversion rate by controlling the water content in a reaction mixture. The method comprises the steps of: preparing a first mixture; producing a second mixture; heating the second mixture; producing a third mixture; analyzing the conversion rate; and adding water to the third mixture when the conversion rate is less than 97 wt%.(AA) Signal 1(BB) Retention time display [min](CC) Area [uV*sec](DD) Height [uV](EE) Area% component name [%](FF) Unidentified component 1(GG) Unidentified component 2(HH) Unidentified component 3(II) Unidentified component 4(JJ) Unidentified component 5(KK) Unidentified component 6(LL) Unidentified component 7COPYRIGHT KIPO 2020
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Paragraph 0058-0063; 0071-0073

(2019/10/17)

Method for Refining Alkyl 3-Alkoxy Propionate
The present invention relates to a method for refining alkyl 3-alkoxy propionate, and more particularly, to a method for refining ethyl 3-ethoxypropionate. According to the method for refining alkyl 3-alkoxy propionate according to the present invention, by continuously refining a reaction production liquid, in which an alkyl 3-alkoxy propionate synthesis reaction using a strong base catalyst is completed, with a high purity by fractional distillation without a neutralization process, it is possible to produce alkyl 3-alkoxy propionate with good solubility that can be used in a semiconductor manufacturing process.(AA) Low boiling organic matter(BB) Low boiling point impurity(CC) Alkyl 3-alkoxy propionate(DD) Moisture-added reaction product(EE) First distillation column(FF) Second distillation column(GG) Third distillation column(HH) High boiling point impurities and nonvolatile ionic impurities(II) Alkyl 3-alkoxy propionate containing mixture(JJ) High boiling point impurityCOPYRIGHT KIPO 2020
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Paragraph 0093-0103

(2020/03/05)

MANUFACTURING METHOD OF N-SUBSTITUTED (METH)ACRYLAMIDE
To provide a method for industrially manufacturing high purity β-alkoxypropionic acid amide, β-aminopropionic acid amide and N-substituted (meth)acrylamide at high yield using (meth)acrylic acid ester as a starting material.SOLUTION: By conducting an amidation reaction with amine in the presence of a metal complex as a catalyst using β-substituted propionic acid ester which is a product material of a Michael addition reaction of (meth)acrylic acid ester and alcohol or amine, β-substituted propionic acid amide is obtained. Further by conducting a thermal decomposition reaction of the β-substituted propionic acid amide in the presence of the metal complex, and eliminating the alcohol or the amine, objective compound N-substituted (meth)acrylamide is obtained.SELECTED DRAWING: None
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Paragraph 0049; 0052

(2019/05/25)

METHOD FOR PRODUCING β-ALKOXYPROPIONIC ACID ESTER
PROBLEM TO BE SOLVED: To provide a method for producing β-alkoxypropionic acid ester, which enables efficient and easy recovery of a product from a reaction mixture obtained by using an alkali metal alkoxide or an alkaline earth metal alkoxide as a catalyst. SOLUTION: The method for producing a β-alkoxypropionic acid ester comprises reacting an alkyl acrylate and alcohols in the presence of an alkali metal or alkaline earth metal alkoxide as a catalyst. After completion of the reaction, a compound which neutralizes the alkali metal or alkaline earth metal alkoxide is added to the reaction mixture, followed by distillation. SELECTED DRAWING: None COPYRIGHT: (C)2018,JPOandINPIT
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Paragraph 0025-0028

(2018/05/03)

Ethyl 3-ethoxypropionate preparation method
The invention discloses an ethyl 3-ethoxypropionate preparation method, wherein the raw materials comprise anhydrous ethanol and ethyl acrylate, and the catalyst is ethyl acrylate accounting for 0.1-20% of the weight. According to the present invention, the method has advantages of simple synthesis, mild conditions, less side reactions, substantially-simplified separation process, convenient continuous production and the like, wherein the catalyst can be recycled without the damage, and can be regenerated.
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Paragraph 0042-0050

(2018/10/19)

MANUFACTURING METHOD OF β-SUBSTITUTED PROPIONIC ACID AMIDE AND N-SUBSTITUTED (METH)ACRYLAMIDE
PROBLEM TO BE SOLVED: To provide a method for industrially manufacturing β-alkoxy propionic acid amide, β-amino propionic acid amide and N-substituted (meth)acryl amide using (meth)acrylic acid ester as starting material at high yield and high purity. SOLUTION: There is provided a method for obtaining N-substituted (meth)acryl amide represented by target compound formula (7) by conducting an amidation reaction with amine using β-substituted propionic acid ester represented by the formula (1) of a product of a Michael addition reaction of (meth)acrylic acid ester and alcohol or amine in presence of a metal complex as a catalyst to obtain β-substituted propionic acid amide represented by the formula (3) and conducting a thermal decomposition reaction of β-substituted propionic acid amide in presence of the metal complex as the catalyst to eliminate alcohol or amine. A-CH2-C(R1)H-C(=O)-OR2 (1), A-CH2-C(R1)H-C(=O)-N(R3)R4 (3), CH2=C(R1)-C(=O)-N(R3)R4 (7) SELECTED DRAWING: None COPYRIGHT: (C)2018,JPOandINPIT
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Paragraph 0046; 0048; 0050

(2018/07/03)

Catalytic Olefin hydroalkoxylation by nano particles of pollucite
The catalytic hydroalkoxylation of α,β-unsaturated esters, nitriles, and ethers with aliphatic and aromatic alcohols over pollucite using thermal and microwave-assisted methods was investigated. To study the effect of the alcohol structures on the mechanism of the hydroalkoxylation reaction, different alcohols, such as methanol to butanol, cyclohexanol, phenol, and 2-ethylhexanol were used. The activities of pollucite, in contrast to other basic solids, were scarcely affected by the presence of air and moisture. The correlation between alcohol acidity and reaction activity is discussed. The prepared pollucite was characterized by X-ray diffraction, volumetric nitrogen adsorption surface area analysis, and CO2 temperature-programmed desorption. Scanning electron microscopy analysis revealed that the size of the modified nano catalyst particles was under 40nm.
Zamanian, Sara,Kharat, Ali Nemati
p. 981 - 986
(2015/06/25)

Oxa-Michael addition promoted by the aqueous sodium carbonate
An efficient Michael addition of alcohols to activated alkenes promoted by sodium carbonate with water as reaction medium has been developed. The reaction provides a general, economical and environmentally friendly approach for the synthesis of β-alkoxycarbonyl compounds.
Guo, Shi-Huan,Xing, Sheng-Zhu,Mao, Shuai,Gao, Ya-Ru,Chen, Wen-Liang,Wang, Yong-Qiang
supporting information
p. 6718 - 6720
(2014/12/11)

Addition of alcohols to acrylic compounds catalyzed by Mg-Al LDH
This study reports the preparation of hydrotalcite with Mg/Al molar ratio 3 by co-precipitation under low suprasaturation conditions of Mg and Al nitrated solutions with Na2CO3 and NaOH at pH 10. The solid was thermally decomposed at 460°C in air atmosphere in order to obtain mixed oxides which, by means of memory effect, can reconstruct the hydrotalcite structure by hydration with bidistilled water. The hydrotalcite and reconstructed samples by memory effect were characterized by elemental analysis, powder XRD, DRIFT and TG-DTG. Determination of the catalysts surface base sites was made using a method based on the irreversible adsorption of organic acids with different pKa values and N2 adsorption-desorption isotherms. The catalytic activity of these solids was evaluated in 1,4-addition of saturated linear alcohols to different acrylic compounds. All these reactions arose with high selectivity in the desired product. No by-products were detected by means of GC-MS chromatography and 1H NMR.
Teodorescu,Deaconu,Bartha,Z?voianu,Pavel
p. 117 - 122
(2014/03/21)

Consecutive Michael-claisen process for cyclohexane-1,3-dione derivative (CDD) synthesis from unsubstituted and substituted acetone 1
A long-existing problem of cyclohexane-1,3-dione derivatives (CDD) synthesis from unreactive acetone through consecutive Michael-Claisen process was solved under this study. The practical applicability of this process was tested for a novel compound ethyl 3-(2,4-dioxocyclohexyl)propanoate for up to 20-gram scale. Furthermore, the scope of different acetone derivatives was investigated and resulted with similar consecutive Michael-Claisen process for CDD synthesis. The reaction exhibited remarkable regioselectivity in Michael addition followed by Claisen cyclization. In this process high substrate selectivity was observed for CDD synthesis following consecutive double-Michael-Claisen and Michael-Claisen cyclization. Georg Thieme Verlag Stuttgart · New York.
Sharma, Dharminder,Shil, Arun K.,Singh, Bikram,Das, Pralay
supporting information; experimental part
p. 1199 - 1204
(2012/06/15)

Heck reactions catalyzed by Pd(0)-PVP nanoparticles under conventional and microwave heating
Pd(0) nanoparticles stabilized by polyvinylpyrrolidone (Pd-PVP) with a diameter of 3-6 nm in ethanol catalyzed Heck coupling of iodobenzene with different alkenes under microwave heating. Products were obtained in good yields (62-99%) and good selectivity to the E-isomers. Microwave heating proved to be superior to conventional heating, providing products in higher yields and selectivities in short times (12 min).
Martins, Daniela De L.,Alvarez, Heiddy M.,Aguiar, Lúcia C.S.,Antunes, Octavio A.C.
scheme or table
p. 47 - 53
(2012/04/11)

Pd(II)-catalyzed acetalization of terminal olefins with electron-withdrawing groups in supercritical carbon dioxide: selective control and mechanism
Pd(II)-catalyzed acetalization of terminal olefins with electron-withdrawing groups was carried out smoothly in supercritical carbon dioxide under oxygen atmosphere when polystyrene-supported benzoquinone (PS-BQ) or CuII (CuI) chloride was employed as cocatalyst. The higher selectivity was achieved, without any chlorinated by-product detected, when using PS-BQ instead of CuII (or CuI) chloride. PS-BQ could be recycled with excellent catalytic activity remaining after each simple filtration. Chlorine ion was demonstrated to be a promoter. The different acetalization mechanisms were revealed by the subtle relationship of chlorine ion and benzoquinone (BQ) to the catalytic activity of PdCl2/PS-BQ, PdII-CuCl2 or Pd(OAc)2/PS-BQ.
Wang, Zhao-Yang,Jiang, Huan-Feng,Ouyang, Xiao-Yue,Qi, Chao-Rong,Yang, Shao-Rong
p. 9846 - 9854
(2007/10/03)

Highly efficient KF/Al2O3-catalyzed versatile hetero-Michael addition of nitrogen, oxygen, and sulfur nucleophiles to α,β-ethylenic compounds
The first example of KF/Al2O3-catalyzed versatile hetero-Michael addition reaction of nitrogen, oxygen, and sulfur nucleophiles was developed for facile preparation of organic compounds of widely different structures. In contrast with the existing methods using many acidic catalysts, this method is very general, simple, high-yielding, environmentally friendly, and oxygen and moisture tolerant.
Yang, Lei,Xu, Li-Wen,Xia, Chun-Gu
p. 3279 - 3282
(2007/10/03)

Novel amine-catalysed hydroalkoxylation reactions of activated alkenes and alkynes
Substoichiometric loadings of DBU catalyse the efficient 1,4-addition of alcohols and non-nucleophilic amines such as pyrrole to activated alkenes; the application of this methodology in a one-pot synthesis of a natural product, and as a novel strategy for the synthesis of mono-protected 1,3-carbonyl compounds is reported.
Murtagh, Julie E.,McCooey, Seamus H.,Connon, Stephen J.
p. 227 - 229
(2007/10/03)

METHODS OF MANUFACTURING DERIVATIVES OF β-HYDROXYCARBOXYLIC ACIDS
Preparation of derivatives of β-hydroxycarboxylic acid, including β-hydroxycarboxylic acid esters, α,β-unsaturated carboxylic acids, esters of α,β-unsaturated carboxylic acid, and alkoxy derivatives.
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Page/Page column 14-15

(2008/06/13)

Revisiting [3 + 3] route to 1,3-cyclohexanedione frameworks: Hidden aspect of thermodynamically controlled enolates
We have revisited the traditional consecutive Michael-Claisen [3 + 3] process (MC-[3+3]) promising the synthesis of a cyclohexane-1,3-dione derivatives from nonactivated simple ketones and enoates and evaluated its potential in modern organic synthesis. Twenty to thirty examples were demonstrated to be effective. The reactions exhibited remarkable regioselectivity with the Michael addition proceeding through nucleophilic attack by the more hindered site of the ketones without exception. The subsequent Claisen condensation resulted in the formation of carbon-carbon bonds between less hindered site of the ketones and acyl carbon of the enoates. The MC-[3+3] process described is useful for the synthesis of Taxol A-ring synthons in multigram quantities and for the synthesis of other six-membered carbocyclic compounds. A number of control experiments have been conducted to provide strong support for the mechanism of this MC-[3+3].
Ishikawa, Teruhiko,Kadoya, Ryuichiro,Arai, Masaki,Takahashi, Haruka,Kaisi, Yumi,Mizuta, Tomohiro,Yoshikai, Kazusa,Saito, Seiki
p. 8000 - 8009
(2007/10/03)

Alkoxide-induced reactions of N-substituted saccharins. Synthesis of 1,2-benzothiazocine 1,1-dioxide and 2,3-dihydropyrrolo[1,2-b]-[1,2]benzisothiazole 5,5-dioxide derivatives
The reactions of saccharin derivatives 1 with sodium alkoxides were studied. Under mild conditions, compounds 1a-f gave the corresponding open sulfonamides 5a-f. Under drastic conditions, β-(saccharin-2)propionic acid derivatives 1a,b reacted with sodium ethoxide affording saccharin and β-ethoxypropionic acid derivatives 4a,b. γ-(Saccharin-2)butyric acid derivatives 1c,d and γ-(saccharin-2)butyrophenone 1f reacted with sodium t-butoxide in dimethyl sulfoxide affording 5-substituted 6-hydroxy-3,4-dihydro-2H-1,2-benzothiazocine 1,1-dioxides 9. From mother liquors, 1-substituted 2,3-dihydropyrrolo[1,2-b][1,2]benzisothiazole 5,5-dioxides 10 were isolated several hours later, though not detected immediately after completing the reaction. When the reactions were carried out in t-butyl alcohol, the yields of 9 diminished and those of 10 increased with product ratio inversion. Different expermental observations on the possible pathway generating 9 and 10 are discussed.
Blanco,Perillo,Schapira
p. 145 - 154
(2007/10/02)

Process for the preparation of alkyl 3-alkoxypropionates
Disclosed is an improved process for the preparation of alkyl 3-alkoxypropionates by the reaction of a dialkoxymethane with a diketene in the presence of methanedisulfonic acid, methanetrisulfonic acid or mixture thereof.
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(2008/06/13)

The reaction of potassium tetracarbonylhydridoferrate with ethyl acrylate in ethanol
The reaction of KHFe(CO)4 with an excess of ethyl acrylate in ethanol for 30 h at 70 deg C leads to ethyl propyonate (270percent with respect to iron) and diethyl 4-oxopimelate (40percent yield with respect to iron), whether in an atmosphere of CO or argon.These reactions are shown to proceed by regioselective addition of KHFe(CO)4, to ethyl acrylate to give an intermediate alkyl tetracarbonylferrate 2 (M=K), which has been isolated as the PPN+ salt.In situ protonation of 2 (or of the isomeric alkyltetracarbonylferrate 10) by the solvent, and reductive elimination of ethyl propionate generate a coordinatively unsaturated Fe(CO)4 species which, when quenched in situ, gives the corresponding Fe(CO4)(acrylate) complex 9.In the presence of K2CO3 and an excess of ethyl acrylate, 9 affords ethyl propionate in 120percent yield with respect to iron, which is consistent with observed pseudo-catalytic reduction of ethyl acrylate by KHFe(CO)4.The formation of diethyl oxopimelate is thought to involve the isomerisation of 2, followed by reaction of the resulting alkyltetracarbonylferrate 10 with ethyl acrylate.
Brunet, Jean-Jacques,Passelaigue, Elisabeth
p. 203 - 216
(2007/10/02)

Process for the preparation of alkyl 3-alkoxypropionates
Disclosed is an improved process for the preparation of alkyl 3-alkoxypropionates containing at least seven carbon atoms by the reaction of dialkoxymethane containing five or more carbon atoms with a ketene in the presence of a catalytic amount of the reaction product of an alkylcarboxylic acid anhydride and concentrated or fuming sulfuric acid.
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(2008/06/13)

The Reaction of Alkyl 3-Alkoxy-2-bromopropanoate with Triethyl Phosphite
Alkyl 3-alkoxy-2-bromopropanoate reacted with triethyl phosphite to give alkyl 2,3-bis(diethoxyphosphinyl)propanoate as the major product.
Okamoto, Yoshiki,Tone, Tsutomu,Sakurai, Hiroshi
p. 303 - 304
(2007/10/02)

Phase-Transfer Catalyzed Reactions. 5. Dramatic Effect of the Concentration of Base on the Dimerization of Crotonaldehyde
Self-condensation of crotonaldehyde under base-catalyzed phase-transfer conditions leads to aldehydes 3 or 4, depending only on the concentration of aqueous hydroxide used.Quaternary ammonium fluorides in anhydrous THF is shown to be a useful system for conjugate additions involving base-sensitive aldehydes.
McIntosh, John M.,Khalil, Hamdy,Pillon, David W.
p. 3436 - 3439
(2007/10/02)