HRID630460

反应详情

EQUATION

反应方程式

HRID 630460 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of m-chloroperoxybenzoic acid (77%, 2.10 g, 9.42 mmol) in dichloromethane (20 mL) was added at 0° C. to (1-(5-bromopyrimidin-2-yl)-3-(methylthio)-1H-indol-6-yl)(morpholino)methanone (0.18 g, 0.25 mmol) in dry dichloromethane (300 mL). The mixture was stirred at room temperature for 4 h and then poured onto saturated sodium sulfite solution (20 mL). The organic layer was separated after stirring for 15 min and washed with saturated sodium hydrogen carbonate solution and brine. The organic phase was then dried over sodium sulphate and concentrated. The residue was purified by flash column chromatography [methanol/dichloromethane=1:40]. White solid. Yield: 3.2 g.

WORKUP

后处理

  1. customThe organic layer was separated
  2. stirringafter stirring for 15 min
  3. washwashed with saturated sodium hydrogen carbonate solution and brine
  4. dry with materialThe organic phase was then dried over sodium sulphate
  5. concentrationconcentrated
  6. customThe residue was purified by flash column chromatography [methanol/dichloromethane=1:40]