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Preparation method of bethanechol chloride

A technology of bethanechol chloride and methylcholine chloride, which is applied in the field of preparation of bethanechol chloride, can solve the problems of high cost, low yield and high pollution of the synthesis process, and achieve The effect of low cost, high yield and simple preparation process

Inactive Publication Date: 2014-07-23
HENAN LINGXIAN SCI & TECHN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the above-mentioned traditional synthesis process has high cost, high pollution and low yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] A preparation method for bethanechol chloride, comprising the steps of:

[0016] a. First add chloroform into the reaction kettle, then add methylcholine chloride, control the temperature at 0°C, add solid phosgene in batches while stirring, the mixture of methylcholine chloride and solid phosgene The ratio of quantity is 1:2;

[0017] b. After each addition of solid phosgene, stir for 5 minutes and then add an equal proportion of the catalyst. After the addition, the temperature is raised to 50° C., and the reaction is for a period of 3 hours, wherein the catalyst is selected from dimethylformamide (DMF), pyridine or triethylamine. In any one, the consumption of described catalyst is 1% of methylcholine chloride weight;

[0018] c. After the reaction is completed, the temperature of the reaction solution is lowered to 15°C;

[0019] d, add the ammoniacal liquor of its weight 20% in the reaction solution, adjust pH value 8, concentrate under reduced pressure to drynes...

Embodiment 2

[0022] A preparation method for bethanechol chloride, comprising the steps of:

[0023] a. First add chloroform into the reaction kettle, then add methylcholine chloride, control the temperature at 40°C, add solid phosgene in batches while stirring, the mixture of methylcholine chloride and solid phosgene The ratio of quantity is 1:2.9;

[0024] b. After each addition of solid phosgene, stir for 10 minutes, then add an equal proportion of catalyst, heat up to 80°C after addition, and react for a period of time for 8 hours, wherein the catalyst is selected from dimethylformamide (DMF), pyridine or triethylamine In any one, the consumption of described catalyzer is 5% of methylcholine chloride weight;

[0025] c. After the reaction is completed, the temperature of the reaction solution is lowered to 25°C;

[0026] d, add its weight 30% ammoniacal liquor in the reaction solution, adjust the pH value to 10, concentrate under reduced pressure to dryness, add dehydrated alcohol wi...

Embodiment 3

[0029] A preparation method for bethanechol chloride, comprising the steps of:

[0030] a. First add chloroform into the reaction kettle, then add methylcholine chloride, control the temperature at 20°C, add solid phosgene in batches while stirring, the mixture of methylcholine chloride and solid phosgene The ratio of quantity is 1:2.5;

[0031] b. After each addition of solid phosgene, stir for 8 minutes and then add an equal proportion of catalyst, heat up to 65°C after addition, and react for a period of 6 hours, wherein the catalyst is selected from dimethylformamide (DMF), pyridine or triethylamine In any one, the consumption of described catalyzer is 3% of methylcholine chloride weight;

[0032] c. After the reaction is completed, the temperature of the reaction solution is lowered to 20°C;

[0033] d, add the ammoniacal liquor of its weight 25% in the reaction solution, adjust pH value 9, concentrate under reduced pressure to dryness, add the dehydrated alcohol of 4 t...

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PUM

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Abstract

The invention relates to a preparation method of bethanechol chloride. The preparation method comprises the following steps: a, firstly adding trichloromethane to a reaction kettle, then adding methylcholine chloride, controlling the temperature at 0-40 DEG C and adding triphosgene stage by stage while stirring; b, adding an isometric catalyst after stirring the materials for 5-10 minutes after adding triphosgene each time and raising the temperature to 50-80 DEG C after adding the catalyst to react for 3-8 hours; c, after reaction is completed, reducing the temperature of the reaction liquid to 15-25 DEG C; d, adding ammonia water which accounts for 20-30wt% of the reaction liquid to the reaction liquid, adjusting the pH value to be 8-10, concentrating the solution at reduced pressure until the solution is dry, adding absolute ethyl alcohol 3-5 times methylcholine chloride by weight and carrying out centrifugal filtration, thus obtaining a crude product of bethanechol chloride; e. adding absolute ethyl alcohol 1-5 times the crude product of bethanechol chloride by weight and activated carbon which accounts for 2-4wt% of the crude product of bethanechol chloride to the crude product of bethanechol chloride, carrying out decoloration, filtration, cooling and recrystallization, carrying out spinning filtration and drying the filter cake, thus obtaining the fine product of bethanechol chloride. The preparation method has the beneficial effects of simple preparation process, low cost, no pollution and high yield.

Description

technical field [0001] The present invention relates to a kind of production method of medicine, particularly a kind of preparation method of bethanechol chloride. Background technique [0002] Saikeling (bethanechol chloride), a cholinergic drug, has the functions of stimulating smooth muscle, promoting gastrointestinal peristalsis, promoting secretion of body fluids, increasing appetite and helping digestion. Saikeling is used for digestive system diseases such as slack stomach, rumen food accumulation, and dry large intestine of ruminants such as cattle and sheep. Stomach dilatation, food accumulation, flatulence, constipation, and nodules in horses; large intestine dryness, gastrointestinal discomfort, and loss of appetite caused by high fever diseases in pigs, the effect is remarkable. It also has significant curative effect on the bladder, urine and retained placenta of various animals. [0003] The traditional synthetic process of bethanechol chloride (commonly know...

Claims

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Application Information

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IPC IPC(8): C07C271/12C07C269/00
Inventor 郭有钢贺国超刘裕东刘占领
Owner HENAN LINGXIAN SCI & TECHN PHARMA