HRID2374478

反应详情

EQUATION

反应方程式

HRID 2374478 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-(1-ethyl-3,3-dimethyl-5-nitro-2-oxo-2,3-dihydro-1H-indol-6-yl)-acetamide (5.2 g, 17.85 mmol) was dissolved in ethanol (40 ml). After addition of hydrochloric acid (25%, 8 ml, 81.44 mmol) the mixture was stirred under reflux for 3 h. The reaction mixture was allowed to cool down to room temperature and then quenched with water (80 ml). The yellow precipitate was isolated by suction and washed with ethanol/water (1:1). The solid was dissolved in ethyl acetate, dried over sodium sulfate and concentrated to yield 4.15 g (93%) 6-amino-1-ethyl-3,3-dimethyl-5-nitro-1,3-dihydro-indol-2-one as a orange solid.

WORKUP

后处理

  1. temperatureunder reflux for 3 h
  2. customquenched with water (80 ml)
  3. customThe yellow precipitate was isolated by suction
  4. washwashed with ethanol/water (1:1)
  5. dissolutionThe solid was dissolved in ethyl acetate
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated