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1-(吡啶-3-基)乙酮与离子液体[bmim]Br_3常温发生溴化反应,然后与硫氰酸铵发生取代反应,再与2-甲基-5-硝基苯胺在乙酸作用下加成环化“一锅法”得到4-(吡啶-3-基)-2-[(2-甲基-5-硝基苯基)氨基]噻唑,进而在Pd-Fe/TiO_2催化下常压氢化得到马赛替尼关键中间体4-(吡啶-3-基)-2-[(2-甲基-5-氨基苯基)氨基]噻唑,总收率为87%。方法简便,收率高,离子液体[bmim]Br_3的反应产物[bmim]Br可用作后续反应的催化剂和溶剂,且可回收利用。
Bromination reaction of 1- (pyridin-3-yl) ethanone with ionic liquid [bmim] Br_3 at room temperature followed by displacement reaction with ammonium thiocyanate followed by reaction with 2-methyl-5-nitroaniline under the action of acetic acid Addition of cyclization “one-pot method” gave 4- (pyridin-3-yl) -2 - [(2-methyl-5-nitrophenyl) amino] Under normal pressure, the key intermediate of 4- (pyridin-3-yl) -2 - [(2-methyl-5-aminophenyl) amino] thiazole was obtained. The total yield was 87%. The method is simple and the yield is high. The [bmim] Br, the reaction product of ionic liquid [bmim] Br_3, can be used as catalyst and solvent for subsequent reaction and can be recycled.