HRID2236581
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionadded dropwise to the reaction mixture over 20 minutes
- filtrationMixture is filtered through celite