2-乙酰基-3-甲基-5-(N-甲苯氨基)噻唑的合成  

Synthesis of 2-Acetyl-3-methyl-5-(N-methylanilino)thiazole

作　　者：陈兆斌[1] 陈淑丽[1] 别红彦[1] 

机构地区：[1]山西大学化学化工学院,山西太原030006

出　　处：《精细化工》2003年第4期193-194,共2页Fine Chemicals

基　　金：国家自然科学基金(30000112);山西省归国留学人员科研基金(晋留2001-1)资助项目

摘　　要：N 甲基苯胺与盐酸及硫氰酸钾回流反应5h,然后用水重结晶得到了N 甲基 N 苯基硫脲,产率40%。将2,4 戊二酮分散到四氯化碳-水的混合溶液中,然后将溴的四氯化碳溶液在1h内滴加到上述溶液中,控制温度为0℃,搅拌45min后,分离出四氯化碳层并蒸去四氯化碳,得到油状物,即为3 溴 2,4 戊二酮,产率79%。3 溴 2,4 戊二酮及N 甲基 N 苯基硫脲溶于丙酮中,回流30min,冷却,然后用碳酸钠溶液碱化,再用乙酸乙酯萃取,蒸去乙酸乙酯就得到2 乙酰基 3 甲基 5 (N 甲苯氨基)噻唑,产率62%。NMethylaniline was refluxed with aqueous HCl and KSCN for 5 h and then recrystallized in water to give NmethylNphenylthiourea(Ⅰ) in 40% yield.A solution of Br2 in CCl4 was added during 1 h to a stirred dispersion of 2,4pentanedione in CCl4-H2O at 0 ℃.After stirring for 45 min,the CCl4 layer was separated,and evaporated to give oily 3bromo2,4pentanedione (Ⅱ) in 79% yield.A solution of Ⅰ and Ⅱ in acetone was refluxed for 30 min,cooled,basified with Na2CO3 solution,and extracted with ethyl acetate.After evaporation to remove ethyl acetate,2acetyl3methyl5(Nmethylanilino)thiazole was obtained in 62% yield.

关 键 词：2-乙酰基-3—甲基—5-(N-甲苯氨基)噻唑 噻唑环 俘精酸酐 合成 

分 类 号：TQ252.5[化学工程—有机化工]