HRID324514

反应详情

EQUATION

反应方程式

HRID 324514 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Concentrated hydrochloric acid (140μL) was added to a solution of the nitrobenzamide, V.3 (147 mg, 0.30 mmol) in methanol (2 ml). Iron (72 mg) was added and the reaction mixture was heated to 80° C. for 2 hours, before cooling. The reaction mixture was basified (saturated sodium carbonate solution), extracted into ethyl acetate, dried over magnesium sulphate and the solvent removed in vacuo to yield an off-white solid which was purified using flash chromatography(ethyl acetate) to yield the desired 2-aminobenzamide, VI.3 (47 mg, 34%).

WORKUP

后处理

  1. temperaturebefore cooling
  2. extractionextracted into ethyl acetate
  3. dry with materialdried over magnesium sulphate
  4. customthe solvent removed in vacuo
  5. customto yield an off-white solid which
  6. customwas purified