Synthesis method of vinpocetine
A technology of vinpocetine and its synthetic method, which is applied in the field of vinpocetine synthesis, can solve the problems of toxicity, high yield, and non-environmental protection, and achieve the effects of high product purity and yield, short reaction steps, and low environmental pollution
Active Publication Date: 2014-05-07
JIANGSU QINGJIANG PHARMA
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The Mondelo patent reports that Vinpocetine is synthesized by using vinblastine as a raw material, acetonitrile as a solvent, and 2-fluoro-1,3,5-trinitrobenzene as a catalyst. The yield of this method is high, but the catalyst is rare and difficult. Realize industrialization, and using acetonitrile as a solvent is very toxic and not environmentally friendly
Kuge et al. used vincamine as a raw material to obtain vincamine ethyl ester through Ti(OEt)4 catalyzed transesterification, and then catalyzed dehydration with methanesulfonic acid to obtain vinpocetine. This method provides ideas for the large-scale production of vinpocetine, but The total yield is not high
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[0019] Step 1: Add the raw material Changchun amine (500g, 1.41mol) to a three -mouth bottle of 5L, then add toluene (2L), stir in the ice water bath, add triplerine (244.4g, 2.42mol), 10 minutes laterSlowly add MSCL (176.8g, 1.55mol), stir in the ice water bath for 2 hours, slowly heat up to room temperature, and continue to stir for 5 hours; the point of the panel is detected, the raw materials are completely transformed, the reaction is stopped, the solvent is directly steamed, the ethanol and water are added to the water and water and water.(2000ml: 200ml), adjust the pH = 12 with a saturated potassium carbonate solution. At this time, there are a large number of solids, filtering directly, vacuum drying, and obtaining Changchun Xiting intermediate (578.6g, 1.33mol), the income rate reaches 95%;
[0020] Step 2: Add water -free ethanol (3L) to a three -mouth bottle of 5L, stir in the ice water bath for 1 hour, slowly add ethanol sodium (180g, 2.66mol), stir 0.5 hours, add Chan...
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The invention discloses a synthesis method of vinpocetine, comprising the following steps: adding vincamine into a three-opening bottle, subsequently, adding methylbenzene, stirring and dropwise adding triethylamine and methylsufonyl chloride in an ice-water bath, slowly heating to room temperature after stirring for 2 h, then continuously stirring for 5 h; stopping reaction, drying solvent by distillation, adding ethanol and water, regulating pH to 12 with saturated potassium carbonate solution, separating out solids, filtering, and drying in vacuum to obtain vinpocetine intermediate; adding absolute ethyl alcohol into the three-opening bottle, stirring in ice-water bath for 1 h, then slowly adding sodium ethoxide, stirring for 0.5 h, then adding the vinpocetine intermediate, subsequently, putting a reaction bottle into an oil bath, setting temperature as 80 degrees centigrade, evaporating most of solvent after reacting for 12 h, then pouring solution into hydrochloric acid, extracting with ethyl acetate, regulating pH to 12 with water phase, separating out solids, filtering and drying to obtain the vinpocetine. According to the synthesis method provided by the invention, reaction steps are short; purity and yield of products are high; energy consumption is low; and environmental pollution is less.
Description
Technical field [0001] The present invention involves the synthesis method, which specifically involves a synthesis method of Changchun Xiting. technical background [0002] VINPOCETINE is a derivative obtained by transforming the vinionic alkaloids from the chipped chypeee churchehumhrine. It is an excellent cerebrovascular disease drug.Changchun Xiting has the ability to increase red blood cell deformation, improve blood fluidity, improve microcirculation, reduce blood viscosity and inhibit platelet condensation, and have the supply of increased and improved brain oxygen.Brain metabolism.It has been widely used abroad for ischemic hypertrophic brain disease, cerebral arteriosclerosis, local arechemia, intermittent cerebral blood flow supply, cerebral vascular spasm, early cerebral enditis, cerebral embolism, cerebral thrombosis, dizziness, dizzinessThe treatment of diseases such as aphasia and Menier syndrome, and has the effects of improving memory, vision, and elderly hearing...
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IPC IPC(8): C07D461/00
Inventor 马玉恒王伟顾海成
Owner JIANGSU QINGJIANG PHARMA