Novel preparation method of palmatine

A technology for compounds and medicinal salts, applied in a new field of salt preparation, can solve problems such as destruction of natural resources

Inactive Publication Date: 2013-01-16
SHANGHAI YIZHI MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, medicinal palmatine is still prepared by the old method of extraction and

Method used

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  • Novel preparation method of palmatine
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  • Novel preparation method of palmatine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The preparation of formula III compound:

[0020] Add 5.2 grams of berberine hydrochloride (HPLC detection content is 98.1%), N, N-dimethylformamide 60ml, phosphorus tribromide 3.5 grams respectively in the reaction flask while stirring slowly, be heated up to 75 ℃ React for 2.5 hours. The reaction solution was lowered to room temperature, and stood for a whole day and night, and the precipitated product crystals were filtered out and dried to obtain the compound of formula III.

Embodiment 2

[0022] The preparation of palmatine hydrochloride:

[0023] After preparing the compound of formula III according to Example 1, add the compound of formula III to the reaction flask with 60 ml of methanol added, heat to dissolve the compound of formula III, add 8.5 grams of sodium methylate, and heat up to the reflux of the reaction solution at a medium speed Stirring was continued for 5.5 hours. The temperature of the reaction solution is lowered to room temperature, left standing for a day and night, and the crystallization (compound of formula IV) of the product is filtered out, and this product is added to the reaction flask having added 80% ethanol 80ml, and the reaction solution is heated while stirring until The solid is completely dissolved, and hydrochloric acid is added to adjust the pH value to 2-3. After standing for a day and night, yellow needle crystals are separated out, filtered off, dried, recrystallized, and dried to obtain 4.9 grams of palmatine hydrochlori...

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Abstract

The invention relates to a novel preparation method of palmatine.

Description

technical field [0001] The invention relates to the fields of organic chemistry and medicinal chemistry, in particular to a new preparation method of palmatine or a pharmaceutically acceptable salt thereof. Background technique [0002] At present, medicinal palmatine is still prepared by the old method of extraction and separation of plant medicinal materials, which has caused serious damage to natural resources. It is urgent to invent a chemical synthesis method to prepare palmatine. Chinese invention patent CN100999522B describes a method for preparing palmatine with berberine. Contents of the invention [0003] The invention discloses a method for preparing a compound (formula III) by using berberine (formula I) and / or berberine salt (formula II), and then converting the compound (formula III) into palmatine (formula IV) or A new preparation method of its pharmaceutically acceptable salt (formula V). Surprisingly, the disadvantages of various existing preparation me...

Claims

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Application Information

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IPC IPC(8): C07D455/03
Inventor 不公告发明人
Owner SHANGHAI YIZHI MEDICAL TECH
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