HRID390125

反应详情

EQUATION

反应方程式

HRID 390125 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Compound 21a (11.8 g, 32.0 mmol) and pyridine (27 ml, 305 mmol) were dissolved in DCM (200 ml) and cooled to 0° C., 4-nitrobenzoyl chloride (6.6 g, 35.6 mmol) was added and the solution was stirred at room temperature overnight. The reaction mixture was washed with NaHCO3 (aq), aqueous citric acid and brine, dried over MgSO4 and evaporated on silica. The crude product was purified by column chromatography on silica (EtOAc/n-Heptane: 50:50) to give 11.84 g, 72% of the title compound.

WORKUP

后处理

  1. washThe reaction mixture was washed with NaHCO3 (aq), aqueous citric acid and brine
  2. dry with materialdried over MgSO4
  3. customevaporated on silica
  4. customThe crude product was purified by column chromatography on silica (EtOAc/n-Heptane: 50:50)