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Method for efficiently preparing propacetamol hydrochloride for injection

A technology for propatamole hydrochloride and injection, which is applied in the field of medicine, can solve the problems of product yield and purity, long reaction and production cycle, low acetone solubility, etc., and achieves shortening production cycle, reducing reaction time, and omitting heavy lifting. Effects of crystallisation operations

Pending Publication Date: 2020-06-12
HAINAN JINXING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method of propatamol hydrochloride for injection uses acetone as lysozyme at present, is acylation catalyst with potassium carbonate, reacts with potassium iodide as ammoniation catalyst, and this method has been able to obtain higher recovery rate and purity, but this method There are problems such as the low solubility of acetone to potassium carbonate, difficulty in removing potassium chloride, etc., and low catalytic efficiency, so the reaction and production cycle is relatively long
If the time of reaction is directly shortened, the yield and purity of the obtained product will be greatly affected, which is obviously not advisable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A kind of method for efficiently preparing propatamol hydrochloride for injection comprises the following steps:

[0021] Take 85 parts by weight of paracetamol, 30 parts by weight of PEG-4000, 240 parts by weight of sodium lactate, and 500 parts by weight of ethanol, adjust the pH to 7.8, mix and stir (800rpm) for 15 minutes, and add 70 parts by weight of chloroacetyl chloride dropwise at 30°C, 10 After the dropwise addition is completed within ~20min, add 60 parts by weight of glycerin, 3 parts by weight of sodium carbonate and 90 parts by weight of diethylamine, mix and stir (800rpm) for 15min; The flow rate of the macroporous resin is 100mL / min); the product is mixed and stirred (800rpm) and added dropwise with hydrogen chloride ethanol solution to pH 3.5 (completed within 5-10min), suction filtered, and the resultant is vacuum-dried to obtain the finished product.

[0022] The types of macroporous resins are D900, D113, D4006 and XAD-4, which are used in combinatio...

Embodiment 2

[0025] A kind of method for efficiently preparing propatamol hydrochloride for injection comprises the following steps:

[0026] Take 85 parts by weight of acetaminophen, 30 parts by weight of PEG-4000, 240 parts by weight of sodium lactate, and 500 parts by weight of ethanol, adjust the pH to 7.2, mix and stir (600rpm) for 30min, add dropwise 70 parts by weight of chloroacetyl chloride at 30°C, 10 After the dropwise addition is completed within ~20min, add 80 parts by weight of glycerin, 3 parts by weight of sodium carbonate and 90 parts by weight of diethylamine, mix and stir (600rpm) for 30min; The flow rate of the macroporous resin is 100mL / min); then the product is mixed and stirred (600rpm) with hydrogen chloride ethanol solution dropwise to pH 3.5 (within 5-10min), suction filtered, and the resultant vacuum-dried to obtain the finished product.

[0027] The types of macroporous resins are D900, D113, D4006 and XAD-4, which are used in combination with a mass ratio of 6:...

Embodiment 3

[0030] A kind of method for efficiently preparing propatamol hydrochloride for injection comprises the following steps:

[0031] Take 80 parts by weight of acetaminophen, 20 parts by weight of PEG-4000, 200 parts by weight of sodium lactate, and 400 parts by weight of ethanol, adjust the pH to 7.8, mix and stir (600rpm) for 30min, add 85 parts by weight of chloroacetyl chloride dropwise at 20°C, 10 After the dropwise addition is completed within ~20min, add 60 parts by weight of glycerin, 5 parts by weight of sodium carbonate and 70 parts by weight of diethylamine, mix and stir (600rpm) for 30min; The flow rate of the macroporous resin is 100mL / min); then the product is mixed and stirred (600rpm) within 5 to 10 minutes to add hydrogen chloride ethanol solution dropwise to pH 1.0, suction filtered, and the resultant is vacuum-dried to obtain the finished product.

[0032] The macroporous resin models are D900, D113, D4020 and XAD-4, which are used in combination, and the mass r...

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PUM

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Abstract

The invention provides a method for efficiently preparing propacetamol hydrochloride for injection. The method mainly comprises the following steps: taking 80-85 parts by weight of acetaminophen, 20-30 parts by weight of PEG-4000, 200-240 parts by weight of sodium lactate and 400-500 parts by weight of ethanol, adjusting the pH value to 7.2-7.8, mixing and stirring for 15-30 minutes, dropwise adding 70-85 parts by weight of chloroacetyl chloride at 20-40 DEG C, after completion of dropwise adding, adding 60-80 parts by weight of glycerol, 3-5 parts by weight of sodium carbonate and 70-90 partsby weight of diethylamine, and mixing and stirring for 15-30 minutes; treating with macroporous resin; and adding 400-500 parts by weight of ethanol, mixing and stirring to dissolve the ethanol, dropwise adding a hydrogen chloride ethanol solution under mixing and stirring until the pH value is 1.0-3.5, carrying out suction filtration, and carrying out vacuum drying on the obtained product to obtain the finished product. According to the method, the propacetamol hydrochloride for injection can be rapidly and efficiently produced on the basis of keeping good recovery rate and purity.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular to a method for efficiently preparing propatamol hydrochloride for injection. Background technique [0002] Propacetamol Hydrochloride is a prodrug of acetaminophen, its chemical name is diethylaminoacetate-4-(acetamido)phenyl hydrochloride, and it is mainly used for the symptomatic treatment of pain, especially in surgical operations Posterior pain and cancer pain. The preparation method of propatamol hydrochloride for injection uses acetone as lysozyme at present, is acylation catalyst with potassium carbonate, reacts with potassium iodide as ammoniation catalyst, and this method has been able to obtain higher recovery rate and purity, but this method There are problems such as the solubility of acetone to potassium carbonate is not high, potassium chloride is difficult to remove, and the catalytic efficiency is not high, so the reaction and production cycle are longer. If the ...

Claims

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Application Information

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IPC IPC(8): C07C231/12C07C231/24C07C233/25
CPCC07C231/12C07C231/24C07C233/25
Inventor 刘全胜刘春燕廖欣国邢贞凯邱燕萍
Owner HAINAN JINXING PHARMA