HRID746773

反应详情

EQUATION

反应方程式

HRID 746773 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Dissolve 4-bromo-3-nitro-benzoic acid methyl ester (4.25 g, 16.3 mmol) in ethanol (100 ml) and water (30 ml). Add sodium dithionite (15 g, 75 mmol) in a single portion and heat the mixture under reflux for 4 h. Evaporate ethanol and add water. Basify the aqueous layer with 10% sodium carbonate solution. Extract the product with EtOAc (×2). Dry the combined organic layers over anhydrous sodium sulfate, filter and concentrate to yield 3-amino-4-bromo-benzoic acid methyl ester (51%).

WORKUP

后处理

  1. temperatureunder reflux for 4 h
  2. extractionExtract the product with EtOAc (×2)
  3. dry with materialDry the combined organic layers over anhydrous sodium sulfate
  4. filtrationfilter
  5. concentrationconcentrate