HRID1602103

反应详情

EQUATION

反应方程式

HRID 1602103 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 4-(imidazol-1-yl)nitrobenzene (89.60 g, 0.474 mol) and 10% palladium on carbon (4.50 g) in ethanol (1200 ml) and 5N HCl (189 ml) was hydrogenated in two batches at 40 psi for 80 minutes. Water (450 ml) was then added to dissolve the product and the catalyst was removed by filtration. washing with more water, and the combined filtrates were evaporated in vacuo, using finally a freeze drier, to give 105.4 g (96%) of the title compound as a cream solid. δH (250 MHz, D2O) 7.22 (2H, d, J=8.8 Hz), 7.35 (1H, t, J=2.1 Hz), 7.44 (2H, d, J=9.0 Hz). 7.59 (1H, t, J=1.8 Hz), 8.89 (1H, t, J=1.5 Hz).

WORKUP

后处理

  1. dissolutionto dissolve the product
  2. customthe catalyst was removed by filtration
  3. washwashing with more water
  4. customthe combined filtrates were evaporated in vacuo