882645-09-2Relevant articles and documents
A cardiovascular drug fasudil hydrochloride intermediate simple synthesis of process
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Paragraph 0019; 0020, (2019/05/15)
The invention discloses a cardiovascular drug fasudil hydrochloride intermediate simple synthesis process, taking ethylenediamine, BOC anhydride, DCM into the reaction bottle stirring, GC to intermediate state the reaction is complete, the reaction solution is concentrated under reduced pressure, concentrate, tetrahydrofuran to stir until completely dissolved, addition of sodium methoxide, thermal insulation stirring [...] 1, 3 - dibromo propane, thermal insulation to stir until the reaction is complete, the reaction solution is poured into ice water, extracted with ethyl acetate twice, combined with the organic phase, a washed, dried with anhydrous sodium sulfate, concentrated under reduced pressure to dry, taking concentrated intermediate, 40% sodium hydroxide, ethanol into the reaction bottle stirring, the reaction solution is heated to reflux, thermal insulation reaction to intermediate state hydrolysis, reverse the ice water, for two armor uncle ether extraction, the combined organic phase, a washed, dried with anhydrous sodium sulfate, concentrated under reduced pressure to dry, adding hexane stirring crystallization, to obtain the product, yield 87.0%, GC99%, raw materials of this invention is simple and easy, the product has high purity, simple and convenient operation, the work efficiency is high.
