HRID618668

反应详情

EQUATION

反应方程式

HRID 618668 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

A mixture of 5-(1-imidazolyl)-2-nitrobenzonitrile (2.14 g), hydrazine hydrate (2 ml), ethanol (25 ml) and DMA (10 ml) was stirred and heated to 40° C. Raney nickel (0.6 g) was added in portions whilst maintaining the temperature at 40-50° C. The mixture was stirred at 40-50° C. for 2 hours. The Raney nickel was filtered off, the mixture was evaporated and the residue was triturated with ethyl acetate (10 ml) to give 2-amino-5-(1-imidazolyl)benzamide (2.03 g); NMR Spectrum: (CD3SOCD3) 6.70 (s, 2H), 6.79 (d, 1H), 7.03 (s, 1H), 7.2 (s, 1H), 7.37 (s, 1H), 7.55 (s, 1H), 7.71 (d, 1H), 7.73 (s, 1H), 8.02 (s, 1H);

WORKUP

后处理

  1. temperaturewhilst maintaining the temperature at 40-50° C
  2. stirringThe mixture was stirred at 40-50° C. for 2 hours
  3. filtrationThe Raney nickel was filtered off
  4. customthe mixture was evaporated
  5. customthe residue was triturated with ethyl acetate (10 ml)