HRID13171

反应详情

EQUATION

反应方程式

HRID 13171 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A mixture of 2-fluoromethoxybenzaldehyde (2.1 mmol, 320 mg), 4-fluorophenylhydrazine hydrochloride (2.1 mmol, 340 mg) and cesium carbonate (3 mmol, 2.0 g) in NMP (6 ml) was heated in a microwave reactor (300 W, 20 min, 150° C.). After cooling to r.t. the reaction mixture was diluted with dichloromethane (20 ml) and washed with 1M HCl, and sat. NaHCO3. The organic layer was dried over Na2SO4, concentrated, and purified by flash chromatography on silica gel (heptane-ethyl acetate).

WORKUP

后处理

  1. temperatureAfter cooling to r.t. the reaction mixture
  2. washwashed with 1M HCl, and sat. NaHCO3
  3. dry with materialThe organic layer was dried over Na2SO4
  4. concentrationconcentrated
  5. custompurified by flash chromatography on silica gel (heptane-ethyl acetate)