HRID743693

反应详情

EQUATION

反应方程式

HRID 743693 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 4-(N-tert-butyloxycarbonyl-N'-piperazinyl)-1-nitrobenzene (3.09 g) in ethanol (70 ml) was hydrogenated at 30 psi for 15 min, in the presence of a palladium on carbon catalyst (0.35 g, 11% (w/w)). The catalyst was filtered off and the residue evaporated in vacuo. The resultant oil was azeotroped with toluene (2×20 ml) followed by petrol (60/80) (20 ml) to afford the aniline (1.96 g). 1H NMR (360 MHz, CDCl3) δ 1.48 (9H, s), 2.96-2.98 (4H, m), 3.56-3.59 (4H, m), 6.65 (2H, d, J=8.7), 6.81 (2H, d, J=8.7 Hz). MS (CI, NH3) 278 (M+1).

WORKUP

后处理

  1. filtrationThe catalyst was filtered off
  2. customthe residue evaporated in vacuo
  3. customThe resultant oil was azeotroped with toluene (2×20 ml)