主要用于医药领域相关研究(基于参考文献中多次出现的医药化学研究背景)
医药
合成路线 1(1. 合成:80360-20-9)
产率:97%
合成条件:Stage #1: With sodium hydride In tetrahydrofuran; mineral oil at 20℃; Cooling with ice Stage #2: at 20℃;
实验步骤:将NaH(60%在矿物油中的分散体,40.00mmol,0.96g)分批加入搅拌的吲哚-3-甲醛11(20.00mmol,2.90g)在无水THF(50mL)中的溶液中,在冰浴中冷却,然后缓慢 允许温暖到rt 搅拌30分钟后,滴加PhSO 2 Cl(24.00mmol,4.24g)的无水THF溶液。 当TLC监测显示原料11已消失时,将反应混合物减压蒸发除去溶剂,然后用冰水(300mL)稀释。 滤出固体产物,用丙酮/石油醚(60-90℃)重结晶,得到所需中间体12,产率97%,熔点151-153℃.1H NMR(600MHz,CDCl3):δ:7.37( t,J = 7.2Hz,1H),7.42(dd,J = 11.4,4.2Hz,1H),7.52(t,J = 7.8Hz,2H),7.62(t,J = 7.2Hz,1H),7.97( t,J = 7.8Hz,3H),8.20-8.31(m,2H),10.11(s,1H)。 HRMS(MALDI):m / z 286.0515。计算。 C 15 H 11 NO 3 S:286.0538 [M + H] +。
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