化学合成。
化学合成
合成路线 1(1. 合成:57332-84-0)
产率:97%
合成条件:With bromine In dichloromethane at 5 - 20℃;
实验步骤:步骤A:3-溴-2-氧代丁酸乙酯(1-B)。向化合物1-A(4.8g,36.9mmol)的CH 2 Cl 2(20mL)溶液中冷却至5℃,加入溴( 滴加1.89mL,36.9mmol)。将反应混合物温热至室温并搅拌18小时。用氮气吹扫反应混合物,用EtOAc稀释,并用10%NaHCO 3洗涤有机相(2 *) ),H 2 O,盐水,用Na 2 SO 4干燥,过滤,减压蒸发溶剂,得到化合物1-B,为黄色油状物(7.50g,97%)。1H-NMR(CDCl3):δ5.15-5.20(q,1H) ),4.32-4.45(m,2H),1.82-1.85(d,3H),1.38-1.41(t,3H)。
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