摘要
以新蒸馏过的环己烯和丙酰氯为原料,与三氯化铝和氟苯一起采用“一锅法”制备4-(4-丙酰基环己基)-氟苯。首先将环己烯与丙酰胺的混合物在搅拌下于-10℃逐滴加入到三氯化铝的氟苯悬浮液中,而后将该反应混合物在40℃下搅拌反应2h即可得4-(4-丙酰基环己基)-氟苯。环己烯、丙酰氯、三氯化铝、氟苯投料摩尔比为1∶1∶1.5∶2。第二步反应是用黄鸣龙法将4-(4-丙酰基环己基)-氟苯还原为4-(反-4-正丙基环己基)-氟苯。最后经减压蒸馏和数次重结晶得到纯度大于99.5%的产品4-(反-4-正丙基环己基)-氟苯。
A new method of synthesis of 4- ( trans-4-n-propylcyclohexyl)-fluorobenzene was described. Two steps that the production of 4-(4-propionylcyclohexyl) -fluorobenzene and its reduction were involved in this method. The first step, a mixture of cyclohexene and propionyl chloride was added dropwise to a suspension of aluminum chloride in fluorobenzene with stirring and cooling to - 10 ℃. The mol ratio of cyclohexene, propionyl chloride, aluminumchloride and fluorobenzene was 1 : 1 : 1.5 : 2. The reaction mixture was stirred subsequently at 40 ℃ for 2 h and the 4- (4-propionylcyclohexyl) -fluorobenzene was gotten.The second step, the 4-(4-propionylcyclohexyl)fluorobenzene was reduced to 4-( trans-4-n-propylcyclohexyl ) -fluorobenzene by HuangMinglong reduction, which was distilled under reduced pressure (0.67--1.33 kPa) and recrystallized several times from ethanol. The pure compound was gotten and the purity was higher than 99.5%.
出处
《化学工程》
EI
CAS
CSCD
北大核心
2005年第4期72-76,共5页
Chemical Engineering(China)
基金
陕西省自然科学基金项目资助(04-5173)
关键词
液晶
环己烯
氟苯
4-(反-4-正丙基环己基)-氟苯
黄鸣龙还原
4-( trans-4-n-propylcyclohexyl ) -fluorobenzene
liquid crystal
cyclohexene
fluorobenzene
HuangMinglong reductive reaction