HRID2236425

反应详情

EQUATION

反应方程式

HRID 2236425 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

3,5-Dimethyl-1-(4-nitro-phenyl)-piperazine (1.40 g, 5.90 mmol) is dissolved in 20 ml of methanol with ˜1 g of Raney nickel suspension. Hydrazine (0.576 g, 14.9 mmol) is dissolved in 20 ml of methanol and added dropwise to the reaction mixture over 20 minutes. Mixture is stirred at room temperature for 3 hours. Mixture is filtered through celite and reduced on rotovap to afford the product as a black solid (1.05 g, 67%); 1H NMR (DMSO-d6) δ 0.94 (d, J=6.3 Hz, 6H), 1.93-2.00 (m, 2H), 2.65-2.85 (m, 3H), 3.13-3.20 (m, 2H), 4.45 (bs, 2H), 6.43 (d, J=8.5 Hz, 2H), 6.61 (d, J=8.5 Hz, 2H).

WORKUP

后处理

  1. additionadded dropwise to the reaction mixture over 20 minutes
  2. filtrationMixture is filtered through celite