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Preparation method of cyclic propyl phosphonic anhydride

A technology of propylphosphonic anhydride and propylphosphonic acid, which is applied in the field of preparation of cyclic propylphosphonic anhydride, can solve the problems that cannot meet the needs of lithium battery additives, is not suitable for industrial production, and the reaction process is easy to get out of control, and achieves low cost , the preparation method is simple, the effect of high reaction yield

Active Publication Date: 2017-08-04
VALIANT CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In the preparation process, after propylphosphonyl chloride and water are combined, a large amount of heat is released, the reaction process is easy to get out of control, and the obtained product contains some polymers, and the obtained product cannot meet the needs of lithium battery additives, nor is it suitable for industrial production.

Method used

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  • Preparation method of cyclic propyl phosphonic anhydride
  • Preparation method of cyclic propyl phosphonic anhydride
  • Preparation method of cyclic propyl phosphonic anhydride

Examples

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Effect test

Embodiment 1

[0041] A preparation method of cyclic propylphosphonic anhydride, the steps are as follows:

[0042] (1) Preparation of propylpyrophosphonic acid: Add 89.0g (720mmol) propylphosphonic acid, 38.8g (380mmol) acetic anhydride and 200mL xylene into a 500mL three-necked flask, fully replace with nitrogen, heat to 128°C, and react for 7.0 h; after completion of the reaction, a vacuum distillation device was installed to evaporate the reaction solvent xylene and by-product acetic acid to obtain 80.2 g of viscous liquid propyl pyrophosphonic acid, with a yield of 96.80%;

[0043] 1 HNMR (400MHz, CDCl 3 ), δ (ppm): 13.262 (s, 2H), 1.836-1.630 (m, 8H) and 1.065-0.996 (m, 6H); 31 PNMR (161.8MHz, CDCl 3 ), δ(ppm): 26.063;

[0044] (2) Preparation of propylphosphonochloride: Add 89.0g (720mmol) propylphosphonic acid, 188.5g (1584mmol) thionyl chloride and 300mL toluene into a 1L three-necked flask, fully replace with nitrogen, heat to 80°C, and react for 4.0 h; After the reaction is c...

Embodiment 2

[0050] A preparation method of cyclic propylphosphonic anhydride, the steps are as follows:

[0051] (1) Preparation of propylpyrophosphonic acid: Add 89.0g (720mmol) propylphosphonic acid, 39.8g (390mmol) acetic anhydride and 200mL toluene into a 500mL three-necked flask, fully replace with nitrogen, heat to 105°C, and react for 8.0h After completion of the reaction, a vacuum distillation device was installed to evaporate the reaction solvent toluene and by-product acetic acid to obtain 79.9 g of viscous liquid propyl pyrophosphonic acid, with a yield of 96.38%;

[0052] 1 HNMR (400MHz, CDCl 3 ), δ (ppm): 13.262 (s, 2H), 1.836-1.630 (m, 8H) and 1.032-0.996 (m, 6H); 31 PNMR (161.8MHz, CDCl 3 ), δ(ppm): 26.331;

[0053] (2) Preparation of propylphosphonochloride: Add 89.0g (720mmol) propylphosphonic acid, 176g (1476mmol) thionyl chloride and 300mL toluene into a 1L three-necked flask, fully replace with nitrogen, heat to 70°C, and react for 6.0h After the completion of the...

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Abstract

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.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a preparation method of cyclic propylphosphonic anhydride. Background technique [0002] Cyclic propylphosphonic anhydride was first used in the synthesis of peptides as a coupling reagent. Later, due to the high activity and unique properties of this compound, it was gradually used in the process of dehydration and coupling reactions between acids and amines in the synthesis of peptides in organic synthesis. Compared with the conventional second-generation condensation reagent (DCC), in addition to higher reaction yield, high purity of crude product and low racemization characteristics, it also has the advantages of low toxicity, good compatibility with functional groups and convenient post-treatment. . In addition, cyclic propylphosphonic anhydride is also widely used in other organic synthesis reactions, and is one of the important means to extend carbon chains and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6571
CPCC07F9/657181
Inventor 林存生邢宗仁刘英瑞石宇胡葆华孟凡民
Owner VALIANT CO LTD
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