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Preparation method of calcium phosphorylcholine chloride

A technology for phosphoryl choline chloride and calcium chloride, which is applied in the field of preparation of calcium phosphoryl choline chloride, and can solve the problems of environmental pollution, difficulty in removing phosphorylation reagents or condensing agents, and easy moisture absorption.

Pending Publication Date: 2021-12-21
TUOXIN GROUP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The raw material in the above process is choline chloride, which is easy to absorb moisture and has strict requirements on the process conditions. The phosphorylation reagent or condensation agent used is difficult to remove in the subsequent steps, which affects the quality of the product and causes serious damage to the environment. Pollution, does not meet the requirements of the modern pharmaceutical industry

Method used

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  • Preparation method of calcium phosphorylcholine chloride
  • Preparation method of calcium phosphorylcholine chloride
  • Preparation method of calcium phosphorylcholine chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] In the reaction flask, add dichloromethane (5mL), triethylamine (0.28mL, 2mmol) and phosphorus oxychloride (0.093mL, 1mmol), cool to -5 ~ 0 ℃ with ice brine, dropwise add ethylene glycol ( 0.056mL, 1mmol), the dropwise addition was completed, stirred and continued to react for 30min, then slowly raised to room temperature, continued to react for 2h, filtered to remove the formed triethylamine hydrochloride, concentrated the filtrate under reduced pressure below 30°C, added toluene to azeotropically remove HCl remained, and 0.135 g of a viscous oil was obtained, namely the intermediate 2-chloro-1,3,2-dioxaphospholane-2-oxide, with a yield of 95%. 1 H NMR (300MHz, CDCl 3 )δ4.41-4.23(m,4H,O-CH 2 -CH 2 -O). 13 CNMR (100MHz, D 2 O) δ71.1.

Embodiment 2

[0030] In the reaction flask, add dichloromethane (50mL), triethylamine (2.78mL, 20mmol) and phosphorus oxychloride (0.93mL, 10mmol), cool to -5 ~ 0 ℃ with ice brine, dropwise add ethylene glycol ( 0.56mL, 10mmol), the dropwise addition was completed, stirred and continued to react for 30min, then slowly raised to room temperature, continued to react for 2h, filtered to remove the formed triethylamine hydrochloride, concentrated the filtrate under reduced pressure below 30°C, added toluene to azeotropically remove HCl remained, and 1.39 g of a viscous oil was obtained, namely the intermediate 2-chloro-1,3,2-dioxaphospholane-2-oxide, with a yield of 98%.

Embodiment 3

[0032] In the reaction flask, add dichloromethane (5mL), triethylamine (0.28mL, 2mmol) and phosphorus oxychloride (0.093mL, 1mmol), cool to -5 ~ 0 ℃ with ice brine, dropwise add ethylene glycol ( 0.028mL, 0.5mmol), the dropwise addition was completed, stirred and continued to react for 30min, then slowly raised to room temperature, continued to react for 2h, filtered to remove the formed triethylamine hydrochloride, concentrated the filtrate under reduced pressure below 30°C, added toluene to azeotrope Residual HCl was removed to obtain 0.067g viscous oil, which was the intermediate 2-chloro-1,3,2-dioxaphospholane-2-oxide compound, yield 95% (taking ethylene glycol as standard calculate).

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Abstract

The invention discloses a preparation method of calcium phosphorylcholine chloride, and belongs to the technical field of medicinal chemistry. The preparation method comprises the following steps: by taking phosphorus oxychloride and ethylene glycol as raw materials, carrying out low-temperature reaction to obtain an intermediate 2-chloro-1,3,2-dioxaphospholane-2-oxide; and reacting the intermediate 2-chloro-1,3,2-dioxaphospholane-2-oxide with trimethylamine to obtain phosphorylcholine, and conducting reacting with calcium chloride to obtain calcium phosphorylcholine chloride. The calcium phosphorylcholine chloride obtained by the method is low in cost and high in purity, many impurities in the traditional method are removed, separation and purification are convenient, and the product quality is reliable.

Description

technical field [0001] The invention belongs to the technical field of medicinal chemistry, and in particular relates to a preparation method of phosphorylcholine calcium chloride. Background technique [0002] Phosphocholine Calcium Chloride, also known as Phosphocholine Chloride Calcium Salt or Phosphocholine Chloride Calcium Salt, English name is Phosphocholine Chloride Calcium Salt, molecular formula: C 5 h 13 NO 4 PCaCl, CAS 4826-71-5, is an important component of phospholipids and lecithin in living organisms, and is the core raw material for the preparation of cytidine diphosphocholine (CDPC for short). Its structural formula is as follows: [0003] [0004] The synthetic method of phosphorylcholine chloride calcium salt reported in the literature is to be starting raw material from choline chloride, react with different phosphorylating reagents to obtain phosphorylcholine chloride, and then react with inorganic calcium salt to convert into chlorine phosphorylch...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/09C07F9/10
CPCC07F9/091C07F9/106
Inventor 杨西宁李涛马冠军吕英杰靳海燕石田清张赛楠
Owner TUOXIN GROUP
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