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二苯氯甲烷的光化学合成
Photochemical Synthesis of Benzhydryl Chloride
【摘要】 以无水氯化锌为催化剂,苯与氯化苄为原料,经Friedel Crafts反应制得二苯甲烷,收率为72 6%;在可见光照射下,二苯甲烷与氯气发生自由基取代反应生成二苯氯甲烷。通过系列实验得出了二苯氯甲烷光化学合成的优化工艺条件:n(二苯甲烷)∶n(氯气)=1∶1 02,光源采用碘钨灯,反应温度90~100℃,通氯时间12h,以二苯甲烷计二苯氯甲烷收率82 2%,产品质量分数≥98%,通过红外和质谱对其结构进行了确证。
【Abstract】 Using anhydrous zinc chloride as catalyst through FriedelCrafts reaction,benzene and benzyl chloride reacted to give diphenylmethane in 726% yield.Then diphenylmethane reacted with chlorine under irradiation of visible light through side chain chlorination to give benzhydryl chloride in 82.2% yield.The optimal conditions for the photochemical reaction were mole ratio of diphenylmethane to chlorine 1∶102,iodinetungsten lamp as light source,reaction temperature 90-100 ℃ and reaction time 12 h.Purity of the product was over 98%(w/w)and its structure was confirmed by IR and MS.
【Key words】 benzhydryl chloride; diphenylmethane; photochemical reaction; pharmic intermediate;
- 【文献出处】 精细化工 ,Fine Chemicals , 编辑部邮箱 ,2003年10期
- 【分类号】O625.1
- 【被引频次】7
- 【下载频次】368