HRID384328

反应详情

EQUATION

反应方程式

HRID 384328 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5-(2-methoxy-3-nitro-phenyl)thiophene-2-carboxylic acid 12a (7.7 g, 27.6 mmol) was dissolved in 300 mL of ethyl acetate followed by addition of 500 mg of palladium on carbon and ammonium formate (6.96 g, 110 mmol). The reaction mixture was heated to reflux for 4 hours. The reaction was monitored by TLC until the disappearance of the starting materials. The mixture was concentrated under reduced pressure and the resulting residue was purified by silica gel column chromatography to obtain the title compound 5-(3-amino-2-methoxy-phenyl)-thiophene-2-carboxylic acid 12b (6.2 g, yield 90.1%) as a grey solid.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 4 hours
  3. concentrationThe mixture was concentrated under reduced pressure
  4. customthe resulting residue was purified by silica gel column chromatography