4206-94-4Relevant academic research and scientific papers
One-pot preparation method of methyl aluminum hypophosphite
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Paragraph 0041-0043; 0054-0057, (2019/02/13)
The invention discloses a one-pot preparation method of methyl aluminum hypophosphite and belongs to the technical field of chemical synthesis. The one-pot preparation method includes: using methanephosphonic dichloride as a raw material to react with water to obtain a methyl hypophosphoric solution; adjusting pH of the methyl hypophosphoric solution to 3/=pH7, adding aluminum sulfate, and allowing reaction to obtain methyl aluminum hypophosphite. The methanephosphonic dichloride is used as a starting material to prepare methyl aluminum hypophosphite by a one-pot process; separating methyl hypophosphoric acid is not required; by controlling water usage, it is possible to avoid side reaction of methanephosphonic dichloride and increase the yield of methyl hypophosphoric acid; by optimizing salt pH, the yield of methyl aluminum hypophosphite is increased. The method has the advantages that the material is low in price and easy to obtain, operation is simple, post-treatment is convenient, and industrial production of methyl aluminum hypophosphite can be achieved.
Preparation method for methylethylphosphinic acid and aluminum salt thereof
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Paragraph 0045-0049; 0053-0057, (2019/10/01)
The invention discloses a preparation method for methylethylphosphinic acid and an aluminum salt thereof, belonging to the technical field of organic synthesis. To reduce the production cost of methylethylphosphinic acid and improve the purity of methylethylphosphinic acid, the invention provides the preparation method for methylethylphosphinic acid and the aluminum salt thereof. The preparation method comprises the following steps: reacting dichloromethylphosphine with water to obtain an aqueous dichloromethylphosphine solution; with di-tert-butyl peroxide as an initiator, reacting the aqueous dichloromethylphosphine solution with ethylene so as to obtain methylethylphosphinic acid; and reacting the methylethylphosphinic acid with an aqueous solution of Al(SO).18HO to obtain the aluminum salt of methylethylphosphinic acid. According to the invention, the aqueous dichloromethylphosphine solution is directly used for preparing the methylethylphosphinic acid, reaction conditions are screened so as to realize high-yield preparation of high-purity methylethylphosphinic acid, and the high-purity methylethylphosphinic acid is directly used for preparing the aluminum salt of methylethylphosphinic acid; so the purification operation of each intermediate is eliminated, which allows production efficiency to be significantly improved and production cost to be reduced.
Synthetic method of methyl hypophosphorous acid monoalkyl ester
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Paragraph 0024; 0026; 0028, (2018/11/22)
The invention discloses a synthetic method of methyl hypophosphorous acid monoalkyl ester and belongs to the technical field of organic synthesis. The invention aims at the problems of low MDP (methylenediphosphonic acid) synthetic yield, strict reaction condition and the like, according to the synthetic method provided by the invention, the methyl hypophosphorous acid monoalkyl ester is producedthrough synthesis of methyl hypophosphorous acid, and the synthesis of MDP is avoided. According to the synthetic method provided by the invention, a common reagent is adopted, methylation is performed firstly, and then esterification is performed to produce the methyl hypophosphorous acid monoalkyl ester. Control points in the entire process are less, technical problems of low yield and the likein a MDP synthesis process can be avoided, a completely new synthetic route of the methyl hypophosphorous acid monoalkyl ester is created, and industrial production is easier to achieved.
PROCESS FOR PREPARING METHYL PHOSPHINIC ACID BUTYL ESTER
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Page/Page column 39; 40, (2018/09/19)
The present subject matter provides a safe alternative for producing an important intermediate useful for preparing the herbicide glufosinate, without need for chlorine components in the manufacturing process. In particular, a process for preparing alkyl phosphinic aid alkyl ester is provided, including the step of alkylating alkyl phosphinic acid ester in a non-polar solvent in the same apparatus as used to first produce the alkyl phosphinic acid ester, and without isolating the alkyl phosphinic acid ester before the alkylation step is conducted. More specifically, a process is presented for preparing methyl phosphinic acid butyl ester, by alkylating butyl phosphinic acid ester in a non-polar solvent, in the same' apparatus as used previously to first produce the butyl phosphinic acid ester and without isolating the butylphosphinic acid ester before alkylation.
Synthesis of new mono- and bisorganophosphorus proline derivatives with P–C–N moieties
Prishchenko, Andrey A.,Livantsov, Mikhail V.,Novikova, Olga P.,Livantsova, Ludmila I.,Petrosyan, Valery S.
, (2017/01/17)
The various methods of aminomethylation of some PH-acids with proline and their derivatives are investigated. The numerous derivatives of proline and corresponding phosphonates, phosphonites, phosphinates, and phosphorane with proline moieties are presented.
Preparation method of monoalkyl hypophosphite
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Paragraph 0027; 0028, (2017/10/10)
The invention relates to a preparation method of monoalkyl hypophosphite. The preparation method is characterized in that a monoalkyl phosphine halate solution is oxidized by dimethyl sulfoxide, wherein the molar ratio of the monoalkyl phosphine halate solution to the dimethyl sulfoxide is 1:2 or 1:2.1; the reaction temperature is between -50 to 20 DEG C; a molecular formula of the monoalkyl hypophosphite is RP(H)OOH, and R is linear and branched alkyl groups with 1 to 6 carbon atom number. The preparation method of the monoalkyl hypophosphite has the advantages that the reaction yield rate is greater than 80%; after reaction is finished, the water and the halogen hydride can be easily separated out through decompression, and then recycled by a sodium hydroxide solution, and the treatment is not used as the main content of the invention, so that the method is safe, environmentally friendly and economic.
Method for preparing monoalkyl hypophosphite
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Paragraph 0027; 0028; 0029, (2017/09/18)
The invention relates to a method for preparing monoalkyl hypophosphite. The method comprises the steps of oxidizing monoalkyl hydrogen phosphide halate solution by virtue of hydrogen peroxide, wherein the molar ratio of the monoalkyl hydrogen phosphide halate solution to hydrogen peroxide is 1 to 2 or 1 to 2.1, and the reaction temperature is between (-50)-(20) DEG C. The molecular formula of monoalkyl hypophosphite is RP(H)OOH, wherein R is C1-C10 straight-chain, branched-chain alkyl groups. The method for preparing monoalkyl hypophosphite has the beneficial effects that the reaction yield is more than 80%, and water and halogen hydride can be easily evaporated at a reduced pressure after the reaction is finished and can be recycled by virtue of a sodium hydroxide solution and are not the main content of the invention, so that the method described by the invention is safe, environment-friendly and economic.
Synthesis of a phosphinate analogue of the anti-tumour phosphate di-ester perifosine via sequential radical processes
Markoulides, Marios S.,Regan, Andrew C.
, p. 119 - 129 (2013/02/23)
An efficient synthesis of a phosphinate analogue of the anti-tumour phosphate di-ester perifosine is described (6 steps and 50% overall yield). The two phosphorus-carbon bonds in the perifosine analogue were prepared by sequential double radical hydrophosphinylation processes. This is the first example of a phosphinate analogue of perifosine, designed to be resistant to hydrolysis by phospholipid-metabolizing enzymes. The Royal Society of Chemistry.
Rapid and efficient synthesis of unsymmetrical phosphinic acids r′t(o)ohr″
Fougere, Cecile,Guenin, Erwann,Hardouin, Julie,Lecouvey, Marc
experimental part, p. 6048 - 6054 (2010/03/02)
A new synthesis of unsymmetrical phosphinic acids R′P(O)OHR″ has been evaluated, The first P-C bond was formed by base-promoted H-phosphinate alkylation of a protected H-phosphinate, which is easier and safer to handle, A onepot methodology was developed for the second P-C bond formation reaction that: involves the sila-Arbuzov reaction. This methodology was then extended to the synthesis of a dialkylphosphinic acid with an amino functionality.
Design, synthesis, and biological evaluation of phosphinopeptides against Trypanosoma cruzi targeting trypanothione biosynthesis
Ravaschino, Esteban L.,Docampo, Roberta,Rodriguez, Juan B.
, p. 426 - 435 (2007/10/03)
As a part of our project aimed at the search for new safe chemotherapeutic and chemoprophylactic agents against American trypanosomiasis (Chagas's disease); a series of phosphinopeptides structurally related to glutathione was designed, synthesized, and evaluated as antiproliferative agents against the parasite responsible for this disease, the hemoflagellated protozoan Trypanosoma cruzi. The rationale for the synthesis of these compounds was supported on the basis that the presence of the phosphinic acid moiety would mimic the tetrahedral transition state of trypanothione synthase (TryS), a typical C:N ligase, and the molecular target of these drugs. Of the designed compounds, 53 and 54 were potent growth inhibitors against the clinically more relevant form of T. cruzi (amastigotes) growing in myoblasts. The efficacy for these drugs was comparable to that exhibited by the well-known antiparasitic agent WC-9. The simple phosphinopeptide structure found as a pharmacophore in the present study constitutes a starting point for the development of straightforward optimized drugs.
