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Method for preparing dimethylamino ethyl bilobalide B by using micro reaction device

A technology of dimethylaminoethyl and micro-reaction devices, applied in the direction of organic chemistry, can solve the problems of high reaction cost, low conversion rate of raw materials, long reaction time, etc., and achieve high conversion rate, simple and efficient process, and stable product quality Effect

Inactive Publication Date: 2016-08-17
NANJING UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The technical problem to be solved in the present invention is to provide a method for preparing dimethylaminoethyl ginkgolide B by using a micro-reaction device, so as to solve the problems in the prior art that the reaction time is long, the conversion rate of raw materials is low, the reaction cost is high and cannot be continued Disadvantages such as chemical preparation

Method used

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  • Method for preparing dimethylamino ethyl bilobalide B by using micro reaction device

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Experimental program
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Effect test

Embodiment 1

[0024] The acetonitrile solution of dimethylaminoethyl chloride hydrochloride (concentration: 0.01g / mL, flow rate: 1mL / min) and the aqueous solution of potassium iodide (concentration: 0.001g / mL, flow rate: 0.1mL / min) were pumped into micro Mixer, then the acetonitrile solution of ginkgolide B (concentration is 0.01g / mL, flow rate is 1mL / min) and the above-mentioned micro-mixer discharge pump into the fixed-bed microwave microreactor filled with potassium carbonate, the ginkgo The mol ratio of lipid B and dimethylaminoethyl chloride ethyl chloride hydrochloride is 1:1, the mol ratio of potassium iodide and ginkgolide B is 0.2:1, and the mol ratio of potassium carbonate and ginkgolide B is 1.5:1, Keep the reaction residence time for 0.5 min, react at 50°C, filter the crude product, concentrate the filtrate, and recrystallize the obtained solid with methanol to obtain dimethylaminoethyl ginkgolide B with a yield of 85%.

Embodiment 2

[0026] Acetonitrile solution of dimethylaminoethyl chloride hydrochloride (concentration: 0.03 g / mL, flow rate: 2 mL / min) and aqueous solution of potassium iodide (concentration: 0.0025 g / mL, flow rate: 1 mL / min) were pumped into micro-mixing device, then the acetonitrile solution of ginkgolide B (concentration is 0.04g / mL, flow rate is 5mL / min) and the above-mentioned micro-mixer discharge pump into the fixed-bed microwave microreactor filled with cesium carbonate, ginkgolide The mol ratio of B and dimethylaminoethyl chloride ethane hydrochloride is 1:2, and the mol ratio of potassium iodide and ginkgolide B is 0.5:1, and the mol ratio of cesium carbonate and ginkgolide B is 1.8:1, keeps The reaction residence time was 0.75 min, and the reaction was carried out at 60°C. The crude product was filtered, the filtrate was concentrated, and the obtained solid was recrystallized with methanol to obtain dimethylaminoethyl ginkgolide B with a yield of 92%.

Embodiment 3

[0028] Acetonitrile solution of dimethylaminoethyl chloride hydrochloride (concentration: 0.04g / mL, flow rate: 3mL / min) and potassium iodide aqueous solution (concentration: 0.0025g / mL, flow rate: 0.37mL / min) were pumped into micro Mixer, then the acetonitrile solution of ginkgolide B (concentration is 0.03g / mL, flow rate is 2.9mL / min) and the above-mentioned micro-mixer discharge pump into the fixed-bed microwave microreactor filled with cesium carbonate, ginkgo biloba The molar ratio of lactone B to dimethylaminoethylene chloride hydrochloride is 1:2, the molar ratio of sodium iodide to ginkgolide B is 0.5:1, and the molar ratio of cesium carbonate to ginkgolide B is 1.8 : 1, keep the reaction residence time 0.75min, react at 60°C, filter the crude product, concentrate the filtrate, recrystallize the gained solid with methanol, obtain dimethylaminoethyl ginkgolide B, and the productive rate is 89%.

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Abstract

The invention discloses a method for preparing dimethylamino ethyl bilobalide B by using a micro reaction device. The method comprises the following steps: simultaneously and respectively pumping an organic solvent solution of dimethylamino ethyl chloride hydrochloride and a solution of metallic iodide into a micro mixer, sufficiently mixing, simultaneously and respectively a discharged material and an organic solvent solution of bilobalide B into a fixed bed microwave micro mixer, and enabling the components to react sufficiently, thereby obtaining a product. Compared with the prior art, the method is simple and efficient in process, and moreover continuous production can be achieved. Meanwhile, a product prepared by using the method is stable in quality and relatively high in conversion rate.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a method for preparing dimethylaminoethyl ginkgolide B by utilizing a micro-reaction device. Background technique [0002] Ischemic cardiovascular and cerebrovascular diseases are major diseases with high morbidity and mortality. At present, the most effective treatment is anti-platelet aggregation. However, such drugs are prone to bleeding, and the development of new anti-platelet aggregation drugs that can avoid the risk of bleeding is currently a global research hotspot. As one of the only surviving old tree species of the genus Ginkgo in the Ginkgo family, the leaves and fruits of the Ginkgo tree have important medicinal value. The most studied is Ginkgo biloba extract, which mainly includes flavonoids and ginkgolides. Ginkgolides mainly include ginkgolides A, B, C, J and M monomers, and ginkgolides A and B have a significant effect on the treatment of cardiova...

Claims

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Application Information

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IPC IPC(8): C07D493/22
CPCC07D493/22
Inventor 郭凯秦引林咸漠方正何伟欧阳平
Owner NANJING UNIV OF TECH
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