HRID20329

反应详情

EQUATION

反应方程式

HRID 20329 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Add acetic anhydride (160 mL) to a solution of 1-(3,5-difluorophenyl)-2-nitroethanol (330 g) and 4-dimethylaminopyridine (18 g) in dichloromethane (1000 mL), over 30 minutes and stir the reaction mixture overnight. Dilute with dichloromethane (600 mL) and wash with 2% aqueous hydrochloric acid, saturated aqueous sodium chloride, saturated aqueous sodium bicarbonate, dry (magnesium sulfate) and concentrate. Wash the crude with hexanes to give the desired compound (220 g).

WORKUP

后处理

  1. washwash with 2% aqueous hydrochloric acid, saturated aqueous sodium chloride, saturated aqueous sodium bicarbonate
  2. dry with materialdry (magnesium sulfate)
  3. concentrationconcentrate
  4. washWash the crude with hexanes