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氟苯挂嗪(Ⅰ)为一种新的高效钙阻滞剂。合成(Ⅰ)的重要中间体为双(4—氟苯基)—氯甲烷(Ⅱ)。本文报道(Ⅱ)的合成及其化学结构的确证。文献的工艺易树脂化,产率低和流程长。我们改进反应条件,缩短了反应时间,获得较高收率。(Ⅱ)的合成是用氟苯与四氯化碳籍无水三氯化铝催化后再水解得双(4-氟苯基)甲酮(Ⅲ),为无色鳞片状结晶,m.p.107—8℃产率63.9%。(Ⅲ)用异丙醇铝/异丙醇还原成双(4-氟苯基)甲醇(Ⅳ),为无色针状结晶,m.p.91℃收率90%。(Ⅳ)用浓盐
Flubenzuron (Ⅰ) is a new and effective calcium blocker. The important intermediate for the synthesis of (Ⅰ) is bis (4-fluorophenyl) -chloromethane (Ⅱ). This paper reports the synthesis of (Ⅱ) and the confirmation of its chemical structure. The literature process is easily resinized, with low yields and long runs. We improve the reaction conditions, shorten the reaction time, to obtain higher yields. (Ⅱ) is the synthesis of bis (4-fluorophenyl) methanone (Ⅲ) catalyzed by anhydrous benzene trichloride with fluorobenzene and carbon tetrachloride to give colorless scale-like crystals. Mp 107- Yield 63.9% at 8 ° C. (III) was reduced to bis (4-fluorophenyl) methanol (IV) using aluminum isopropoxide / isopropanol as colorless needles, m.p. 91% yield. (Ⅳ) with concentrated salt