- Synthesis method of 1-propyl phosphoric acid cyclic anhydride
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The invention provides a 1-propyl phosphoric acid cyclic anhydride synthesis method, which comprises: S1, carrying out a chlorination reaction on 1-propyl diethyl phosphate and a chlorination reagentto obtain a 1-propyl phosphorus dichloride intermediate; and S2, heating the 1-propyl phosphorus dichloride intermediate and 1-propyl diethyl phosphate to 100-300 DEG C, and carrying out a cyclizationreaction to obtain the 1-propyl phosphoric acid cyclic anhydride. The embodiment of the invention discloses a synthetic method of 1-propyl phosphoric acid cyclic anhydride. According to the method, diethyl 1-propylphosphate is used as a starting raw material, and chlorination is performed under the action of dichloromethane and thionyl chloride to prepare the 1-propylphosphorus dichloride intermediate, so that the product can be obtained by adopting simple, easily available and cheap raw materials through a two-step reaction, the production cost is low, and the method is suitable for industrial production.
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Paragraph 0055; 0059-0063; 0067-0071; 0075-0079; 0083-0086
(2020/09/16)
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- Preparation method of cyclic propyl phosphonic anhydride
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The invention belongs to the technical field of organic synthesis and particularly relates to a preparation method of cyclic propyl phosphonic anhydride. The method comprises the steps of preparing propyl pyrophosphate from propenylphosphonic acid and acetic anhydride as reactants; preparing propyl phosphonyl chloride from propenylphosphonic acid and thionyl chloride as reactants; carrying out further reaction on the propyl pyrophosphate and the propyl phosphonyl chloride to prepare the cyclic propyl phosphonic anhydride. According to the prepared cyclic propyl phosphonic anhydride, the reaction yield is high and the total yield can reach 68-72%, the cyclic propyl phosphonic anhydride is low in cost and high in purity, the titration purity is greater than 99.5%, the content of free acid is smaller than 100ppm, the polymer content is low, and use of a lithium battery additive can be met. The preparation method is simple, safe, environment-friendly, high in efficiency, cheap and available in raw materials, wide in market prospect and suitable for massive production.
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Paragraph 0046; 0047; 0048; 0055; 0056; 0057
(2017/09/01)
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- An improved 1-propyl phosphonic acid of anhydrides and nitriles preparation method (by machine translation)
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The invention relates to an improved preparation method of 1-propylphosphoric cyclic anhydride, which comprises the following steps: 1) adding dimethylpropyl phosphate into an ionic liquid solvent while controlling the temperature at 0-80 DEG C, adding acetic anhydride at the same technical temperature within 1-3 hours, and heating to react under reflux for 1-8 hours to obtain a reaction solution, wherein the mol ratio of the ionic liquid solvent to the dimethylpropyl phosphate to the acetic anhydride is (10-15):(2.0-2.8):1; 2) after finishing refluxing, distilling the reaction solution at 80-140 DEG C under normal pressure to remove low-boiling-point substances; and 3) carrying out vacuum distillation on the distilled reaction solution at 235-260 DEG C to obtain the 1-propylphosphoric cyclic anhydride. The product prepared by the method is a colorless syrupy thick liquid; the yield is greater than or equal to 93%, and the content is 98-99.5%; and compared with the prior art, the yield and technique are greatly enhanced.
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Paragraph 0024; 0025
(2016/10/07)
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- An optimized and scalable synthesis of propylphosphonic anhydride for general use
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Abstract Propylphosphonic anhydride (T3P) is an effective coupling and dehydrating agent, which has been used for a large number of chemical transformations. An efficient and versatile synthetic method is described to synthesize propylphosphonic anhydride (T3P) in pure form, in an overall yield of 51% in four steps from commercially available diethyl phosphonate.
- Pizova, Hana,Bobal, Pavel
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p. 2014 - 2017
(2015/03/30)
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- PROCESS
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The present invention relates to a process for recovering a phosphonic acid. The present invention also relates to the conversion of a phosphonic acid to a phosphonic acid anhydride.
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Page/Page column 15-16
(2010/04/03)
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- METHOD FOR THE PRODUCTION OF CYCLIC PHOSPHONIC ACID ANHYDRIDES
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Disclosed is a method for producing cyclic phosphonic acid anhydrides of formula (III) by a) reacting phosphonic acid derivatives of formula (I) with acetic anhydride at a temperature ranging between 30 and 150 °C while separating a mixture of ethanoic acid and acetic anhydride by means of distillation, b) then reactively distilling the oligomeric phosphonic acid anhydrides of formula (II) obtained in step a) and transforming the same into the corresponding cyclic trimeric phosphonic acid anhydrides of formula (III), n representing a number between 0 and 300 while R represents allyl, aryl, or open-chain, cyclic, or branched C1 to C8 alkyl radicals, aryloxy, allyloxy, or alkoxy comprising open-chain, cyclic, or branched C1 to C8 alkyl radicals. Preferably, the cyclic trimeric phosphonic acid anhydrides formed in step b) are immediately dissolved in an organic solvent that exhibits an inert behavior relative thereto.
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Page/Page column 8
(2008/06/13)
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