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Synthesis process of phentolamine mesilate

A technology for the synthesis of phentolamine mesylate, which is applied in organic chemistry and other fields, can solve the problem that the pH value index is not easy to control, etc., and achieve the effect of less steps, less impurities and low cost

Inactive Publication Date: 2013-11-27
KUNSHAN SANYOU PHARMA MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the control of chlorides in large-scale industrial production is a relatively troublesome problem, and the index of pH value is not easy to control

Method used

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Examples

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Embodiment 1

[0027] A kind of synthetic technique of phentolamine mesylate, comprises the following steps:

[0028] A neutralization:

[0029] (a1) Add 2500mml of distilled water heated to 65°C into a 4000mml beaker, add 50g of phentolamine hydrochloride into the beaker under stirring, and add 25g of silica gel H for the first time after stirring to dissolve completely, adjust the pH to 7.5 with dilute ammonia water, Then filter to obtain filtrate I;

[0030] (a2) Add 20 g of silica gel H to the filtrate I for the second time, adjust the pH to 8 with dilute ammonia water, and filter to obtain the filtrate II;

[0031] (a3) Add 15g of silica gel H15g to the filtrate II for the third time, adjust the pH to 8.5 with dilute ammonia water, and filter to obtain the filtrate III;

[0032] (a4) Reduce the temperature of the filtrate III to below 30°C, slowly add dilute ammonia water dropwise under stirring until all crystals are precipitated, wait for 1 hour and then filter, rinse with distilled...

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Abstract

The invention discloses a synthesis process of phentolamine mesilate. The synthesis process of the phentolamine mesilate comprises the following steps: A, neutralizing, namely, adjusting phentolamine hydrochloride by using diluted ammonia water for many times under the action of silica gel until proper pH value is achieved, and filtering to obtain filtrate to obtain phentolamine free alkali, watering and washing with distilled water for many times until the filtrate is qualified through chloride tracking detection, and drying and crystallizing to obtain a phentolamine free alkali refined product; and B, salifying namely, adding an ethanol solution of methanesulfonic acid into the phentolamine free alkali refined product dropwise by taking absolute ethanol as a solvent, precisely adjusting the pH value to be 5 to 6, then performing a water bath vacuum distillation salt forming reaction, inoculating ethyl acetate, separating out and crystallizing, washing and drying to obtain the phentolamine mesilate. According to the synthesis process of the phentolamine mesilate, the prominent problems that chloride and pH value are not easy to control during actual production are solved, purity is high and impurities are few.

Description

technical field [0001] The invention relates to a synthesis process of phentolamine mesylate, which belongs to the technical field of chemical synthesis process. Background technique [0002] Phentolamine mesylate is an α-receptor blocking drug. Because it has an exciting effect on the heart and can promote blood vessel expansion, it has been used more and more widely in recent years. There are also many routes and methods for preparation and production. However, the control of chlorides in large-scale industrial production is a more troublesome problem, and the index of pH value is not easy to control. Contents of the invention [0003] Objective: In order to overcome the deficiencies in the prior art, the present invention provides a synthesis process of phentolamine mesylate. [0004] Technical solution: In order to solve the above-mentioned technical problems, the technical solution adopted in the present invention is: [0005] A kind of synthetic technique of phent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/24
Inventor 吴小弟
Owner KUNSHAN SANYOU PHARMA MATERIAL
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