HRID434018

反应详情

EQUATION

反应方程式

HRID 434018 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 5-allyloxy-1-[(2-thiophen-3-yl)ethyl]-1H-indole-2-carboxylic acid ethyl ester (1.36 g, 3.8 mmol) was added a mixture of dichloromethane:morpholine:water (100:10:2, 50 mL) followed by the addition of tetrakis(triphenylphosphine) palladium (0) (300 mg). After stilling at room temperature for 18 h, the reaction was partitioned between dichloromethane and water. The organic layer was washed with HCl (3N), NaHCO3, brine and dried over Na2SO4. Purification by flash column chromatography (silica gel, 10-30% EtOAc/hexanes) yielded the desired product as a off-white solid (1.3 g, 86%).

WORKUP

后处理

  1. customthe reaction was partitioned between dichloromethane and water
  2. washThe organic layer was washed with HCl (3N), NaHCO3, brine
  3. dry with materialdried over Na2SO4
  4. customPurification by flash column chromatography (silica gel, 10-30% EtOAc/hexanes)