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Anisodamine production method

A production method and technology for anisodamine are applied in the production field of anisodamine, can solve the problems of waste, low collection ratio of anisodamine, rough process and the like, and achieve the effect of improving the collection purity

Inactive Publication Date: 2014-11-05
施佩蓓
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current method for preparing anisodamine is due to the roughness of the process, and the collection ratio of anisodamine is relatively low, resulting in a large amount of waste

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] The invention provides a kind of production method of anisodamine, it is characterized in that, comprises the steps:

[0014] S1. Take the coarse powder of scopolamine, add 25% concentration of ammonia water and soak it for 15 minutes;

[0015] S2, add diethoxymethane for percolation, and extract the percolation liquid with 2% sulfuric acid;

[0016] S3, add chloroform to wash, add ammonia water to adjust the pH to 8, add carbon tetrachloride for extraction.

[0017] S4, adding water to wash the carbon tetrachloride layer, then adjusting to a pH value of 9; extracting with chloroform, adding anhydrous sodium sulfate to the chloroform layer to dry;

[0018] S5, chloroform is recovered by filtration, and the residue is dissolved in anhydrous benzene to precipitate crystals;

[0019] S6, add benzene to wash, and dry at 55° C. to obtain anisodamine.

[0020] The collection rate of the invention improves the collection purity of anisodamine, and the purity reaches 95%.

Embodiment 2

[0022] The invention provides a kind of production method of anisodamine, it is characterized in that, comprises the steps:

[0023] S1. Take scopolamine coarse powder, add 26.5% concentration of ammonia water and soak for 17 minutes;

[0024] S2, add diethoxymethane for percolation, and extract the percolation liquid with 2% sulfuric acid;

[0025] S3, add chloroform to wash, add ammonia water to adjust the pH to 8, add carbon tetrachloride for extraction.

[0026] S4, add water to wash the carbon tetrachloride layer, then adjust to pH 9.5; extract with chloroform, add anhydrous sodium sulfate to the chloroform layer to dry;

[0027] S5, chloroform is recovered by filtration, and the residue is dissolved in anhydrous benzene to precipitate crystals;

[0028] S6, add benzene to wash, and dry at 57° C. to obtain anisodamine.

[0029] The collection rate of the invention improves the collection purity of anisodamine, and the purity reaches 97%.

Embodiment 3

[0031] The invention provides a kind of production method of anisodamine, it is characterized in that, comprises the steps:

[0032] S1. Take the coarse powder of scopolamine, add 28% concentration of ammonia water and soak it for 20 minutes;

[0033] S2, add diethoxymethane for percolation, and extract the percolation liquid with 2% sulfuric acid;

[0034] S3, add chloroform to wash, add ammonia water to adjust the pH to 9, add carbon tetrachloride for extraction.

[0035] S4, add water to wash the carbon tetrachloride layer, and then adjust to a pH value of 10; extract with chloroform, and add anhydrous sodium sulfate to the chloroform layer to dry;

[0036] S5, chloroform is recovered by filtration, and the residue is dissolved in anhydrous benzene to precipitate crystals;

[0037] S6, add benzene to wash, and dry at 60° C. to obtain anisodamine.

[0038] The collection rate of the invention improves the collection purity of anisodamine, and the purity reaches 98%.

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PUM

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Abstract

The invention provides an anisodamine production method which comprises the following steps: S1, taking belladonna coarse powder, adding 25% to 28% concentration of ammonia for soaking for 15-20min; S2, adding diethoxymethane for percolation, extracting the percolation liquid with 2% sulfuric acid; S3, adding chloroform for cleaning, adding the ammonia to adjust pH to 9, adding carbon tetrachloride for extraction; S4, adding water for washing carbon tetrachloride layer, and adding anhydrous sodium sulfate into chloroform layer for drying; S5, filtering and recovering the chloroform, adding anhydrous benzene for dissolution, and precipitating crystal; and S6, adding benzene for washing, drying at 55-60 DEG C to obtain anisodamine. The anisodamine production method improves the collection rate and collection purity of the anisodamine, the purity reaches 98%, and the process parameters are optimized.

Description

technical field [0001] The invention relates to a production method of anisodamine, in particular to a production method of anisodamine using coarse powder of anisodamine. Background technique [0002] Anisodamine anticholinergic drug. It can relax smooth muscle and relieve vasospasm, so it has an analgesic effect. There are tablets and injections in the ready-made medicine. Clinically, injections are often used because of poor oral absorption. Anisodamine can be used to treat infectious toxic shock, sciatica, gastric and duodenal ulcers, retinitis pigmentosa and other diseases. Its chemical name is: (±)-6β-hydroxy-1αH, 5αH-tropane-3α-ol tropinate. Chemical structural formula: Molecular formula: C17H23NO4 Molecular weight: 305.38. The current method for preparing anisodamine is due to rough technique, and the collection ratio of anisodamine is relatively low, resulting in a large amount of waste. Contents of the invention [0003] The object of the present invention i...

Claims

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Application Information

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IPC IPC(8): C07D451/10
CPCC07D451/10
Inventor 施佩蓓
Owner 施佩蓓
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