Preparation method of dehydro-harmine

A technology of dehydrohaeline and camel calla, which is applied in the direction of organic chemistry, can solve the problems of low specificity of dehydrohamateline, complicated preparation process, and small preparation amount, and achieve reduction of chloroform extraction times and dosage, preparation Large amount, reduce the effect of oil dissolution

Inactive Publication Date: 2012-07-25
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] As mentioned above, the existing technology has low specificity in the method for preparing dehydrohalpine, the preparation process is complicated, the preparation amount is small, and the yield is low

Method used

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  • Preparation method of dehydro-harmine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Take Camelia seeds, crush them, weigh 200g, add 50ml of 5% ammonia water, mix well and ammonify for 20 hours, add 1000ml of 80% methanol solution to soak for 12 hours, filter, add 600ml of 80% methanol for 2 times, combine the extracts, filter, add 400ml of chloroform solution was stirred, and after standing to separate layers, the chloroform layer was collected, and the chloroform was recovered to obtain 8.2g of solid matter. Take petroleum ether, ethyl acetate, methanol, and water and mix them according to the ratio of 17:29:26:16. Take the upper phase as the stationary phase and inject it into a high-speed countercurrent chromatograph at a speed of 800r / min. The lower phase is the mobile phase with a flow rate of 2ml / min. , dissolving the sample with methanol, injecting the sample to separate the sample, collecting the dehydrohaeline fraction, recovering the reagent, and drying in a vacuum at low temperature to obtain 6.1 g of dehydrohaeline, the content of which was ...

Embodiment 2

[0024] Take Camelia seeds and crush them, weigh 200g, add 40ml of 15% ammonia water, mix well and ammonify for 10 hours, add 1000ml of 80% methanol solution to soak for 15 hours, filter, add 1000ml of 80% methanol for soaking, combine the two extracts, filter, add 450ml of chloroform solution was stirred, and after standing to separate layers, the chloroform layer was collected, and the chloroform was recovered to obtain 9.2g of solid matter. Take petroleum ether, ethyl acetate, methanol, and water and mix them according to the ratio of 17:29:26:16. Take the upper phase as the stationary phase and inject it into a high-speed countercurrent chromatograph at a speed of 850r / min. The lower phase is the mobile phase with a flow rate of 2ml / min. , the sample was dissolved in methanol, the sample was injected to separate the sample, the dehydrohaeline fraction was collected, the reagent was recovered, and dried in a vacuum at low temperature to obtain 6.8 g of dehydrohaeline, the con...

Embodiment 3

[0026] Take Camelia seeds and crush them, weigh 500g, add 100ml of 10% ammonia water, mix well and ammoniate for 15 hours, add 2500ml of 70% methanol solution to soak for 15 hours, filter, add 2500ml of 70% methanol to soak, combine the two extracts and filter, Add 1200ml of chloroform solution and stir, after standing to separate layers, collect the chloroform layer, recycle the chloroform to obtain 31.4g of solid. Take petroleum ether, ethyl acetate, methanol, and water and mix them according to the ratio of 17:29:26:16. Take the upper phase as the stationary phase and inject it into a high-speed countercurrent chromatograph at a speed of 900r / min. The lower phase is the mobile phase with a flow rate of 3ml / min. , dissolving the sample with methanol, injecting the sample to separate the sample, collecting the dehydrohaeline fraction, recovering the reagent, and drying in a vacuum at low temperature to obtain 13.1 g of dehydrohaeline, the content of which was detected by high-...

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Abstract

The invention relates to a preparation method of dehydro-harmine, which comprises the steps of smashing harmel seeds which are taken as a material, adding appropriate ammonia water, mixing uniformly, carrying out ammoniation for 10-20 hours, adding a 70-80% carbinol solution with 3-5 times as quantity as that of the material for soaking for 2-3 times, filtering soaking liquid, adding a chloroform solution, collecting a chloroform layer, recycling the chloroform, carrying out separation preparation on solid by a petroleum ether-ethyl acetate-carbinol-hydrosolvent system through using a high-speed counter current chromatograph, collecting dehydro-harmine fluid, recycling reagents, and drying under a low-temperature vacuum condition, so that pure dehydro-harmine is obtained. The method is applicable to the preparation of the dehydro-harmine with high purify.

Description

Technical field: [0001] The invention relates to a method for preparing dehydrohamateline, in particular to a method for separating and preparing dehydrohamateline by using a high-speed countercurrent chromatograph. Background technique: [0002] Dehydrohalamine is also called harminine, pilocarpine, dehydrohalamine, molecular formula C 13 h 12 N 2 O. [0003] Molecular weight 236.7, structural formula [0004] [0005] Dehydrohalamine also has a strong effect on the central nervous system, cardiovascular system, respiratory system and immune system, and also has anti-cancer, analgesic, anti-inflammatory and anti-fungal, anti-bacterial, anti-viral and anthelmintic effects. [0006] Peganum harmala L., also known as Artemisia camel, bitter bitter vegetable, stinky grass, and stinky peony, is the whole herb of the perennial herb of the genus Peganum of the family ZygopHyllaceae. The whole camel grass contains alkaloids, steroids, flavonoids, anthraquinones, amino acids...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D471/04
Inventor 李法庆刘东锋
Owner 苏州宝泽堂医药科技有限公司
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