HRID47180

反应详情

EQUATION

反应方程式

HRID 47180 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

The nitrophenol (3) (36.0 g, 0.1 mol) was dissolved in ethyl acetate (250 ml) and dimethylformamide (DMF) (50 ml). The solution was hydrogenated over Raney Nickel at 3040 kPa (30 atm)/25 C. for 15 h. The catalyst was removed by filtration through a pad of Kieselguhr and the ethyl acetate removed in vacuo. The residual solution of aminophenol (4) in DMF was poured on to an ice/water mixture (1.51) to precipitate aminophenol (4) (27 g, yield 84%), which was collected by filtration and dried. This was stored under a blanket of nitrogen while the ballast acid chloride was prepared.

WORKUP

后处理

  1. customThe catalyst was removed by filtration through a pad of Kieselguhr
  2. customthe ethyl acetate removed in vacuo
  3. additionThe residual solution of aminophenol (4) in DMF was poured on to an ice/water mixture (1.51)