【摘要】 甲硝唑 85g、乙酸乙酯 5 0 0mL、液溴 2 6mL ,于 0℃滴加三氯化磷 4 4mL ,80℃回流 3h ,减压蒸去溶剂后加水 2 0 0mL ,再用活性炭 2g脱色 ,用NaOH水溶液调节pH值 5～ 6 ,得粗品 ,经乙醇重结晶得产品 93 98g ,产品总收率为 81% ,产品质量分数 99 79%更多还原

【Abstract】 To a stirred solution of 85 g(0 5 moles) 1 hydroxyethyl 2 methyl 5 nitroimidazole and 26ml Br 2 in 500 mL EtOAc which was cooled to 0 ℃ was added 44 mL PCl 3.The reaction mixture was stirred for 3 h at refluxing temperature of 80 ℃.Then the solvent was removed at reduced pressure ,200 mL H 2O was added and the solution was decolored with 2 g active carbon.The aqueous solution was adjusted to pH 5-6 with 5 mol/L NaOH to give the crude product.Recrystallization from EtOH yielded 93 98 g (81%) 1 (2′ bromoethyl) 2 methyl 5 nitroimidazole of 99.79% purity.更多还原