- 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 0055-0058; 0063-0066; 0071-0074; 0079-0082
(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 0044; 0045; 0053; 0054
(2017/09/01)
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- Oral Delivery of Propofol with Methoxymethylphosphonic Acid as the Delivery Vehicle
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Phosphonamidate 3a of methoxymethylphosphonic acid (MMPA) with propofol (1) and l-alanine ethyl ester was found to be an efficient scaffold for the oral delivery of compound 1. The synthesis and evaluation of MMPA based phosphonamidates of compound 1, HSK3486 (2), and other phenolic drugs revealed the general application of MMPA as the effective delivery vehicle for phenolic drugs. On the basis of plasma concentrations of compound 1 and SN38 (14), the oral bioavailability of compound 3a and 15 in beagle dogs was found to be 97.6% and 34.1%, respectively.
- Wei, Yonggang,Qiu, Guanpeng,Lei, Bailin,Qin, Linlin,Chu, Hongzhu,Lu, Yonghua,Zhu, Guozhi,Gao, Qiu,Huang, Qingping,Qian, Guofei,Liao, Pengfei,Luo, Xinfeng,Zhang, Xiaowei,Zhang, Chen,Li, Yao,Zheng, Suxin,Yu, Yan,Tang, Pingming,Ni, Jia,Yan, Pangke,Zhou, Yi,Li, Pan,Huang, Xia,Gong, Aisheng,Liu, Jianyu
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supporting information
p. 8580 - 8590
(2017/11/03)
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- The mechanism of thionyl chloride reaction with dialkyl alkylphosphonothionate using 31P NMR
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Based on 31P NMR studies of thionyl chloride reaction with dialkyl alkylphosphonothionates, a method for preparation of alkylphosphonic dichloride has been investigated. A mechanism via intermediacy of ester chloride is suggested.
- Purnanand,Shakya,Saxena, Shefali,Sharma,Lal, Basant
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p. 1093 - 1099
(2007/10/03)
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- Process for the preparation of phosphonic acid dihalides
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Process for preparing phosphonic acid dihalides of the formula EQU1 wherein R is alkyl of 1 to 18 carbon atoms, cycloalkyl of 4 to 8 carbon atoms, alkenyl of 2 to 18 carbon atoms, phenyl, phenalkyl or alkyl-phenyl of 7 to 8 carbon atoms, phenyl, phenalkyl or alkyl-phenyl of 7 to 8 carbon atoms, all radicals R optionally being substituted by chlorine, bromine, cyano or lower acyloxy, and wherein X is halogen such as 2-chloroethane phosphonic acid dichloride, by reacting phosphonic or thio-phosphonic acids of the formula EQU2 wherein Y is oxygen or sulfur, their salts or functional derivatives, with acid halides of the formula wherein X is chlorine or bromine and n is 1 or 2, in the presence of 0.2 - 5% or in the presence of 0.01 to 0.2% by weight of 1. compounds containing at least one tri- to pentavalent nitrogen or phosphorus atom, which in the case of nitrogen is bound with 1 to 4, in the case of phosphorus with at least 3 valences to organic radicals having up to 20 carbon atoms, two of these valences optionally forming a double bond, or 2. mono-di- or tribasic organic or inorganic fully amidated acids or tri- or pentavalent phosphorus, the N atom of which optionally being substituted by aliphatic radicals having up to 20 carbon atoms, and the organic radicals of which contain up to 20 carbon atoms, If required, in the presence of an inert solvent.
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