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作 者:于海涛[1] 康汝洪[1] 董玉环[2] 朱智甲[1] 甄小丽[3] 韩建荣[1]
机构地区:[1]河北师范大学化学系,河北石家庄050016 [2]唐山师范专科学校化学系,河北唐山063000 [3]河北科技大学基础部,河北石家庄050018
出 处:《精细化工》2000年第2期106-108,共3页Fine Chemicals
基 金:河北省教委基金!资助项目(96221)
摘 要:首次以苯和叔戊醇为基础原料经烷基化、酰基化和关环3 步反应合成了2戊基蒽醌。改进和优化了各步合成工艺条件:在三氯化铝- 硫酸双酸催化下,当n(AlCl3)∶n(H2SO4)= 1∶1-25,n(C6H6)∶n(tC5H11OH) =9∶1,温度6 ℃,反应4 h 时,戊苯收率为79-3% ;在2甲基吡啶存在下,中间体2(4′戊基苯甲酰) 苯甲酸收率为80-2 % ;关环反应采用氯仿为溶剂,利用类似分水器的装置,有效控制反应温度使炭化减少,2戊基蒽醌收率为81-4 % 。Using benzene and tert amyl alcohol as starting materials,a new method for preparation of 2 amylanthraquinone involving Friedel Crafts alkylation,acylation and cyclization was described.In the presence of AlCl\-3 and H\-2SO\-4 catalysts,when the molar ratio of AlCl\-3∶H\-2SO\-4 was 1∶1 25,and C 6H 6∶t C 5H 11 OH was 9∶1, reaction holding at 6 ℃ for 4 h,amylbenzene was obtained in 79 3% yield.In the presence of 2 methylpyridine,the intermediate product 2 (4′ amylbenzoyl)benzoic acid was formed in 80 2% yield. By use of a device similar to water segregator and by controlling the temperature,cyclization of the intermediate product in chloroform reduced carbonization and gave 2 amylanthraquinone in 81.4% yield.
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