HRID1370108

反应详情

EQUATION

反应方程式

HRID 1370108 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-(1,1-dimethyl-2-hydroxyethylamino)-3-nitro-5-(trifluoromethyl)pyridine (1.2 g) in pyridine (12 mL) was added acetic anhydride (0.811 mL), and the mixture was stirred at room temperature under nitrogen atmosphere for 4 hours. The resulting mixture was concentrated in vacuo, and the residue was partitioned between ethyl acetate and water. The separated organic layer was washed successively with 1 N-hydrochloric acid, water, an aqueous saturated sodium hydrogencarbonate solution and brine. The organic layer was dried over magnesium sulfate and evaporated in vacuo to give 2-(2-acetoxy-1,1-dimethylethylamino)-3-nitro-5-(trifluoromethyl)pyridine (1.39 g) as a yellow oil.

WORKUP

后处理

  1. concentrationThe resulting mixture was concentrated in vacuo
  2. customthe residue was partitioned between ethyl acetate and water
  3. washThe separated organic layer was washed successively with 1 N-hydrochloric acid, water
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. customevaporated in vacuo