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    • 3. 发明申请
    • AN IMPROVED PROCESS FOR THE PREPARATION OF TERBINAFINE HYDROCHLORIDE
    • 一种改进的格列本脲氯化氢的制备方法
    • WO2005110968A1
    • 2005-11-24
    • PCT/IN2005/000157
    • 2005-05-13
    • HYDEX CHEMICALS PVT LTD.GUPTA, Rajender, PrashadSEKHAR REDDY, Kaku, Vijay
    • GUPTA, Rajender, PrashadSEKHAR REDDY, Kaku, Vijay
    • C07C209/08
    • C07C209/08C07C211/30
    • The present invention relates to an improved process for preparation of terbinafine hydrochloride ,which is (E) - N- Methyl -N-(1-Naphtylmethyl)-6,6-dimethylhept-2-ene-4-ynyl-1-amine has the formula (I), which comprises reacting t-butylacetylene with ethylmagnesium bromide in THF (ii) adding acrolein at a temperature in the range of 0-10o C to get , 6,6-dimethyl-hept-1-ene-4-yne-3-ol, (iii) reacting it with a mixture of phosphorous oxychloride and hydrochloric acid in methanol (iv) extracting the reaction mass with aliphatic/aromatic solvent & removing the solvent (v) reacting the residue with N-(1-naphtylmethyl)methyl amine in the presence of a base to give Terbinafine (vi) adding hydrochloric acid and extracting the Terbinafine Hcl formed with a chlorinated solvent and (vii) recovering the chlorinated solvent under vacuum and adding ethylacetate to separate Terninafine hydrochloride which is filtered and dried.
    • 本发明涉及一种制备特比萘芬盐酸盐的改进方法,其是(E)-N-甲基-N-(1-萘甲基)-6,6-二甲基庚-2-烯-4-炔-1-胺具有 式(I),其包括使叔丁基乙炔与溴化乙基镁在THF中反应(ii)在0-10℃的温度下加入丙烯醛得到6,6-二甲基 - 庚-1-烯-4-酮 (iii)使其与甲醇中的三氯氧磷和盐酸的混合物反应(iv)用脂族/芳族溶剂萃取反应物质并除去溶剂(v)使残余物与N-(1- 萘基甲基)甲基胺,得到特比萘芬(vi)加入盐酸并萃取由氯化溶剂形成的特比萘芬Hcl,和(vii)在真空下回收氯化溶剂,并加入乙酸乙酯分离经过滤的盐酸泰尼芬铵, 干燥。