HRID280294

反应详情

EQUATION

反应方程式

HRID 280294 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of N,N-dimethyl-2-benzyl-3-(4-trifluoromethylphenoxy)propylamine (22.0 g) and ethyl chloroformate (34.1 g, 30.0 ml) in dry toluene (200 ml) is refluxed for 72 hours. The reaction mixture is cooled to room temperature, and the solvent removed under reduced pressure. Water (200 ml) is added, and the mixture extracted with dichloromethane (2×150 ml). The combined dichloromethane extracts are washed with 2N hydrochloric acid (200 ml) and water (200 ml), and dried over magnesium sulfate. The solvent is removed under reduced pressure to give N-carbethoxy-N-methyl-2-benzyl-3-(4-trifluoromethylphenoxy)propylamine as an oil, which is used without purification for the next synthetic step above.

WORKUP

后处理

  1. customthe solvent removed under reduced pressure
  2. additionWater (200 ml) is added
  3. extractionthe mixture extracted with dichloromethane (2×150 ml)
  4. washThe combined dichloromethane extracts are washed with 2N hydrochloric acid (200 ml) and water (200 ml)
  5. dry with materialdried over magnesium sulfate
  6. customThe solvent is removed under reduced pressure