HRID270698

反应详情

EQUATION

反应方程式

HRID 270698 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of (2,6-dichloro-3-nitro-phenyl)-acetic acid (0.90 g, 3.35 mmol) in thionyl chloride (15 mL) is refluxed for one hour. The solvent is removed by concentration and dry toluene is added to thoroughly remove thionyl chloride. To the solution of acid chloride in dry dichloromethane (30 mL) is added (drop-wise) a solution of 2-aminobenzaldehyde (0.365 g, 3.02 mmol) in dichloromethane (5.0 mL). The mixture is stirred at room temperature for 2 hours. The reaction mixture is diluted with EtOAc and washed with saturated K2CO3 and brine. The organic layer is dried, filtered and concentrated to give crude product (0.94 g, 88.6%).

WORKUP

后处理

  1. customThe solvent is removed by concentration and dry toluene
  2. additionis added to thoroughly remove thionyl chloride
  3. washwashed with saturated K2CO3 and brine
  4. customThe organic layer is dried
  5. filtrationfiltered
  6. concentrationconcentrated