Method for synthesizing creatinol-o-phosphate

A technology of inositol phosphate and synthesis method, which is applied in the field of organic chemical synthesis, can solve the problems of serious environmental pollution, high equipment and operation requirements, and achieve the effects of no environmental pollution, simple and easy operation, and mild process conditions

Active Publication Date: 2012-07-18
JIANGSU YUANYANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method produces a large amount of acid waste liquid in the production process, which seriously pollutes the environment. At the same time, due to the use of phosphorylating agent phosphorus pentoxide, the equipment and operation requirements for the reaction are relatively high.

Method used

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  • Method for synthesizing creatinol-o-phosphate

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preparation example Construction

[0017] A kind of synthetic method of inositol phosphate, comprises the steps:

[0018] (1) Using N-methyl-2-aminoethanol as raw material, reacting with phosphoric acid to prepare N-methyl-2-aminoethanol phosphate;

[0019] (2) React N-methyl-2-aminoethanol phosphate obtained in step (1) with O-methylisourea sulfate under alkaline conditions to prepare inositol phosphate.

[0020] Wherein, in step (1), the molar ratio of N-methyl-2-aminoethanol to phosphoric acid is 1:1-1.1, and the reaction conditions are: reaction temperature 0-180°C, reaction time 2 ~6h, the preferred reaction conditions are: reaction temperature 40~150°C, reaction time 3~5h; in step (2), the N-methyl-2-aminoethanol phosphate and O-methylisourea sulfuric acid The molar ratio of the salt is 1:1-1.1, and the reaction conditions are: reaction temperature 0-60°C, reaction time 1-4h, preferred reaction conditions are: reaction temperature 10-50°C, reaction time 2-3h.

[0021] The chemical equation of this react...

Embodiment 1

[0024] Add 75.8g of methylethanolamine and 100ml of water into a 1000ml four-neck flask, add 99.1g of phosphoric acid dropwise at a temperature of 30°C, raise the temperature to 160°C, concentrate to dryness under reduced pressure, cool down to 90°C, add 200ml of water, and control the temperature to 30°C ℃, add 186g of O-methylisourea sulfate dropwise, after the dropwise addition, keep warm for 3h, adjust the pH of the solution to 7.0 with liquid caustic soda, cool down to 0℃, filter, wash the filter cake with 100ml of ice water, and dry to obtain 155.9g of myo-inositol phosphate, the purity is 99.12%, and the yield is 79.14%.

Embodiment 2

[0026] Add 75.8g of methylethanolamine and 100ml of water into a 1000ml four-neck flask, add 110g of phosphoric acid dropwise at a temperature of 72°C, raise the temperature to 180°C, concentrate to dryness under reduced pressure, cool down to 90°C, add 200ml of water, and control the temperature to 20°C , add 176.5g of O-methylisourea sulfate dropwise, after the dropwise addition, keep warm for 1h, adjust the pH of the solution to 7.0 with liquid caustic soda, cool down to 0°C, filter, wash the filter cake with 100ml of ice water, and dry to obtain 130.2 g inositol phosphate, the purity is 99.34%, and the yield is 66.09%.

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Abstract

The invention discloses a method for synthesizing creatinol-o-phosphate, which comprises the steps as follows: (1) N-methyl-2-amino ethanol is taken as a raw material, and reacts with phosphoric acid so as to obtain N-methyl-2-amino ethanol phosphate ester; and (2) the N-methyl-2-amino ethanol phosphate ester obtained in the step (1) reacts with O-methyl isourea sulfate under an alkaline condition so as to obtain the creatinol-o-phosphate. The method is simple and feasible to operate, technological conditions are mild, the productivity and the purity of the obtained product are high, waste gas and waste acid are not generated during the whole process, the safety of equipment and operating staff are ensured, environment cannot be polluted, economical efficiency is achieved, and the requirements of clean production are satisfied.

Description

technical field [0001] The invention relates to a method for preparing inositol derivatives, in particular to a method for synthesizing inositol phosphate, and belongs to the technical field of organic chemical synthesis. Background technique [0002] Creatinol phosphate (COP for short), chemical name: 1-(2-hydroxyethyl)-1-methylguanidine dihydrogen phosphate, English name: 1-(2-Hydroxyethyl)-1-methylguanidine dihydrogen phosphate , Alias: inositol phosphate. [0003] [0004] Inositol phosphate is an important pharmaceutical intermediate, as a drug, it can be used for sedation, anticonvulsant, antiarrhythmia, treatment of cardiac insufficiency, regulation of osmotic pressure, lowering of blood pressure, treatment of arteriosclerosis, inhibition of central nervous system, maintenance of vision, choleretic , liver protection, detoxification, anti-inflammatory, antipyretic and so on. Inositol phosphate is beneficial to the intellectual development of the human brain, and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/09
Inventor 温建华王建峰任举司双喜顾琦王敏文
Owner JIANGSU YUANYANG PHARMA
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