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Isoforskolin preparing method

A technology for forskolin and isoforskolin, which is applied in the field of preparation of high-purity isoforskolin, can solve the problems of low content of the active ingredient isforskolin, meet the requirements of low reaction conditions and the like, and has high yield , the effect of high crystallization yield

Active Publication Date: 2016-06-22
KUNMING MEDICAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with the wild medicinal materials in Yunnan, the medicinal materials planted in Tongcheng County have no significant difference in pharmacognosy, chemical composition and pharmacology, but the content of the active ingredient isophoreskolin is relatively low

Method used

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  • Isoforskolin preparing method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1 Investigation of reaction conditions

[0025] Using forskolin as raw material, using particle size: 200-400 mesh, pH value (100g / L, 25℃): 9.0-10.0 basic alumina catalyst, choose dichloromethane, tetrahydrofuran, methanol, ethanol, benzene As the reaction solvent, the effect of isoforskolin preparation at room temperature was investigated; the reaction vessel was sealed with nitrogen gas; the acetyl group rearrangement reaction was carried out by mechanical stirring. After the reaction is completed, filter, soak and wash the catalyst with the amount of catalyst (kg): washing solvent (L)=1:1.5 methanol (MeOH), combine the filtrate and distill to obtain the crude product;

[0026] Reaction solvent

[0027] Through the comparison of different solvents, it is found that the reaction solvent has a great influence on the preparation method of the present invention. Tetrahydrofuran, methanol and ethanol are selected as the reaction solvent, and the reaction speed is ver...

Embodiment 2

[0029] The method for preparing Isoforskolin described in this embodiment specifically includes the following steps:

[0030] (1) Forskolin as raw material, particle size: 200-400 mesh, pH value (100g / L, 25°C): 9.0-10.0 basic alumina catalyst, dichloromethane (DCM) solvent;

[0031] (2) Under suitable conditions: ①Raw material dosage: catalyst dosage: solvent dosage=1g:20g:25ml; ②Temperature 15℃; ③Time 48h; ④The reaction vessel is sealed with nitrogen; ⑤The acetyl group is rearranged by mechanical stirring. reaction;

[0032] (3) After completing the reaction, filter, use catalyst amount (kg): washing solvent (L)=1:1.5 methanol (MeOH) to soak and wash the catalyst, combine the filtrate and distill to obtain the crude product;

[0033] (4) Purification by secondary crystallization, the first crystallization purification, the solvent ratio (volume ratio) is ethyl acetate (EA): petroleum ether (PE) = 1:2, the amount of solvent is crude product (kg): crystallization solvent (L)=1:9, heat...

Embodiment 3

[0052] The method for preparing Isoforskolin described in this embodiment specifically includes the following steps:

[0053] (1) Forskolin as raw material, particle size: 200-400 mesh, pH value (100g / L, 25°C): 9.0-10.0 basic alumina catalyst, dichloromethane (DCM) solvent;

[0054] (2) Under suitable conditions: ① Quantity of raw materials: quantity of catalyst: quantity of solvent=1g:20g:25ml; ②temperature 40℃; ③time 72h; ④reaction vessel is sealed with nitrogen; ⑤rearrangement of acetyl groups is carried out by mechanical stirring reaction;

[0055] (3) After completing the reaction, filter, use catalyst amount (kg): washing solvent (L)=1:1.5 methanol (MeOH) to soak and wash the catalyst, combine the filtrate and distill to obtain the crude product;

[0056] (4) Purification by secondary crystallization, the first crystallization purification, the solvent ratio (volume ratio) is ethyl acetate (EA): petroleum ether (PE) = 1:2, the amount of solvent is crude product (kg): crystalliza...

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Abstract

The invention relates to an isoforskolin preparing method. The method comprises the steps of utilizing forskolin as a raw material, utilizing a basic catalyst and a dichloromethane (DCM) solvent to carry out ethanoyl rearrangement reaction in an appropriate condition, filtering after reaction, separating liquid from solid, combining filter liquid, distilling the filter liquid to obtain a crude product and crystallizing and purifying the certain proportion and the certain amount of ethyl acetate (EA) and petroleum ether (PE) to prepare the high-purity isoforskolin with the purity larger than or equal to 99 percent.

Description

Technical field [0001] The present invention relates to a method for preparing isoforskolin, in particular to a method for preparing high-purity isoforskolin (Isoforskolin). Background technique [0002] Studies have shown that Coleus forskohlii (Wild.) Briq, a plant of the labiatae family, is produced in India, Nepal and other countries as well as my country’s Yunnan Huize, Dongchuan and other places. Isoforskolin (Isoforskolin) ) Is represented by half-day antane-type diterpenoids, which have obvious effects on the treatment of bronchial asthma, congestive heart failure, various tumors and other related diseases, and the demand has increased significantly. A lot of work has been done domestically in the purification and extraction of effective ingredients, expanding the scale of planting, and increasing the content of effective ingredients. The Chinese patent document with the patent number 201110458818.4 discloses a method for extracting the active ingredient of Coleus forskoh...

Claims

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Application Information

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IPC IPC(8): C07D311/92
CPCC07D311/92
Inventor 杨为民李鲜翁稚颖宋流东陈晨邹澄吴文娟陈丹
Owner KUNMING MEDICAL UNIVERSITY
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