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Method for preparing phosphorylcholine chloride calcium salt tetrahydrate

A technology for phosphoryl choline chloride calcium salt and tetrahydrate, which is applied in the field of preparation of phosphoryl choline chloride calcium salt tetrahydrate, can solve the problems of many impurities and a large amount of waste water, and achieves high product purity and no The effect of three wastes generation and simple process

Active Publication Date: 2014-07-23
苏州正济药业有限公司
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Problems solved by technology

[0008] The present invention provides a preparation method of phosphorylcholine chloride calcium salt tetrahydrate, the purpose of which is to solve the problem of many impurities in the product and the generation of a large amount of waste water and waste gas in the current preparation method of phosphorylcholine chloride calcium salt , solid waste, etc.

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  • Method for preparing phosphorylcholine chloride calcium salt tetrahydrate

Examples

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Embodiment 1

[0027] Example 1: A preparation method of phosphorylcholine chloride calcium salt tetrahydrate

[0028] Add 1032g of orthophosphoric acid into a 2L four-neck flask, heat it to 160~165°C, add dropwise the mixed clarified solution of 1032g of orthophosphoric acid and 852g of choline chloride, and continue to react at 160~165°C for 2 hours until Anhydrous evaporated. A total of about 520 g of water was collected.

[0029] Transfer the feed liquid into a 50-liter glass reactor. After the temperature drops to 30°C, add 15kg of purified water, stir until the solution is colorless, clear and transparent, and the pH is between 1 and 2, add 520g of calcium chloride, and stir at room temperature until completely dissolved; Slowly add 900g of calcium carbonate, a lot of foam is produced, the feed liquid is white and milky, stir at room temperature for 30min, add calcium hydroxide 540g, stir at room temperature for 30min, keep the pH at 8.0, the feed liquid is white and milky, add 2kg of...

Embodiment 2

[0033] Example 2: A preparation method of phosphorylcholine chloride calcium salt tetrahydrate

[0034] Add 1032g of orthophosphoric acid into a 2L four-neck flask, heat it to 160~165°C, add dropwise the mixed clarified solution of 1032g of orthophosphoric acid and 852g of choline chloride, and continue to react at 160~165°C for 2 hours until Anhydrous evaporated. A total of about 520 g of water was collected.

[0035] Transfer the feed liquid into a 50-liter glass reactor. After the temperature drops to 30°C, add 15kg of purified water, stir until the solution is colorless, clear and transparent, and the pH is between 1 and 2, add 520g of calcium chloride, and stir at room temperature until completely dissolved; Slowly add 900g of calcium carbonate, a lot of foam is produced, the feed liquid is white and milky, stir at room temperature for 30min, add calcium hydroxide 540g, stir at room temperature for 30min, keep the pH at 8.0, the feed liquid is white and milky, add 2kg of...

Embodiment 3

[0039] Embodiment three: a kind of preparation method of phosphorylcholine chloride calcium salt tetrahydrate

[0040] Add 1988g of orthophosphoric acid into a 2L four-neck flask, heat it to 160~165°C, add dropwise the mixed clarified solution of 639g of orthophosphoric acid and 852g of choline chloride, and continue to react at 160~165°C for 2 hours until Anhydrous evaporated. About 503g of water were collected in total.

[0041] Transfer the feed liquid into a 50-liter glass reactor, after the temperature drops to 30°C, add 15kg of purified water, stir until the solution is colorless, clear and transparent, and the pH is between 1 and 2, add 298g of calcium chloride, and stir at room temperature until completely dissolved; Slowly add 1278g of calcium carbonate, a large amount of foam is produced, the feed liquid is white and milky, stir at room temperature for 30min, add calcium hydroxide 670g, stir for 30min at room temperature, keep the pH at 8.0, the feed liquid is white...

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Abstract

The invention relates to a method for preparing phosphorylcholine chloride calcium salt tetrahydrate. The method is characterized by consisting of the following steps: (1) dropwise adding a phosphoric acid solution of anhydrous choline chloride into orthophosphoric acid, and reacting at the temperature of 130-180 DEG C, so as to produce phosphorylcholine chloride; (2) enabling a reaction solution to be subjected to neutralization reaction with a proper amount of calcium chloride, calcium carbonate and calcium hydroxide in water; (3) after neutralization reaction, carrying out solid-liquid separation, and refining filter cakes, so as to obtain calcium dihydrogen phosphate or dicalcium phosphate; (4) filtrating a filtrate, obtained through filtrating, with a filter, and then, concentrating and dehydrating; (5) crystallizing a concentrated solution by adding an alcohol solvent, thereby obtaining the product. The method has the advantages that the process flow is simple, waste gases, waste water and waste residues are not generated, and the product quality meets the requirements of crude drug production.

Description

technical field [0001] The invention belongs to the technical field of medicinal chemistry, and in particular relates to a preparation method of phosphorylcholine chloride calcium salt tetrahydrate. Background technique [0002] Phosphoryl Choline Chloride Calcicam Salt (full name in English: Phosphoryl Choline Chloride Calcicam Salt) is an important component of phospholipids and lecithin in organisms, and is the core raw material for the preparation of cytidine diphosphocholine (CDPC for short). The structural formula is as follows: [0003] [0004] According to the difference of crystal water, there are three structures, one does not contain crystal water, one contains one molecule of crystal water, and one contains four molecules of crystal water; usually, it is used for pharmaceutical raw materials and intermediates. Phosphorylcholine chloride calcium salt with tetramolecular water of crystallization. The quality specifications of phosphorylcholine chloride calciu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/09C01B25/32
Inventor 蒋勇钱超黄兵徐敏
Owner 苏州正济药业有限公司
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