HRID404703

反应详情

EQUATION

反应方程式

HRID 404703 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

2,6-Dimethyl-pyridin-3-ol (3.0 g, 24.35 mmol) and cesium carbonate (15.87 g, 48.71 mmol) were added to a solution of 3,4-difluoronitrobenzene (3.87 g, 24.35 mmol) in DMF (30 ml). The mixture was heated at 140° C. for 2 hours. After cooling to room temperature it was filtered through diatomaceous earth and the solvent evaporated in vacuo. The crude product was purified by column chromatography (silica gel; 2% methanol/DCM as eluent) to yield intermediate D14 (5.88 g, 92%).

WORKUP

后处理

  1. temperatureAfter cooling to room temperature it
  2. filtrationwas filtered through diatomaceous earth
  3. customthe solvent evaporated in vacuo
  4. customThe crude product was purified by column chromatography (silica gel; 2% methanol/DCM as eluent)
  5. customto yield intermediate D14 (5.88 g, 92%)