摘要
以对甲苯胺为起始原料,经氯乙酰化,2-氯-6-氟苯酚醚化、重排,再经氯乙酰化,无水AlCl3催化下环合,最后经开环反应制得氯美昔布,整个反应条件温和,反应总收率达到58.8%。在环合反应中,n(Ⅲ):n(无水AlCl3)=1:1.3:反应时间5h;反应温度165—170℃时,环合反应收率达83.1%。
Lumiracoxib was synthesized by chloroacetylation of p - Toluidine with chloroacetyl chloride, etherincation with 2 - chloro- 6 - fluorophenol and rearragement reaction, then chloroacetylation again, cyclization catalyzed by anhydrous aluminium chloride,and ring opening reaction.The whole course ran smoothly. The overall yield reached 58.8% .Experimental results indicated,the acetamide( Ⅲ )and aluminium chloride in mole ratio 1:1.3 reacted at 165 ~ 170℃ for 5 h to give the cyclization product in 83.1% yield.
出处
《化工时刊》
CAS
2006年第3期46-47,50,共3页
Chemical Industry Times