HRID1457186

反应详情

EQUATION

反应方程式

HRID 1457186 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

A mixture of the title compound of Step (C), 1H-1,2,3-triazole (144 mg, 2.1 mmol) and K2CO3 (1.3 g, 9.5 mmol) in 3.8 ml sulfolane was heated at 140° C. for 3 hrs. After cooling, 30 ml H2O was added and the mixture was extracted with 1:1 EtOAc/hexane. The combined organic extracts were washed with H2O and brine, dried and concentrated. The residue was chromatographed on silica gel using 3:1 hexane/EtOAc to afford the title compound of this step (256 mg, 44% for three steps).

WORKUP

后处理

  1. temperatureAfter cooling
  2. extractionthe mixture was extracted with 1:1 EtOAc/hexane
  3. washThe combined organic extracts were washed with H2O and brine
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was chromatographed on silica gel using 3:1 hexane/EtOAc