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
Trifluoroacetic acid (10 ml) was added to a solution of 1-(tert-butoxycarbonyl)-4-(4-dimethylaminophenyl)piperazine (2.01 g 6.58 mmol) in dichloromethane (20 ml) and the mixture stirred for 30 min at room temperature. The mixture was concentrated in vacuo and saturated aqueous potassium carbonate (100 ml) was cautiously added to the residue. The mixture was extracted with dichloromethane (3×100 ml), the extracts were washed with brine (50 ml), combined and dried (MgSO4). Concentration of the extracts gave 1-(4-dimethylaminophenyl)piperazine (1.14 g, 84%) as a cream solid; δH (DMSO-d6) 2.77 (6H, s, N(CH3)2), 2.79 (4H, m, 2×piperazinyl CH2), 2.86 (4H, m, 2×piperazinyl CH2), 2.86 (4H, m, 2×piperazinyl CH2), 6.68 (2H, m, ArH), and 6.82 (2H, m, ArH).
WORKUP
后处理
- concentrationThe mixture was concentrated in vacuo and saturated aqueous potassium carbonate (100 ml)
- additionwas cautiously added to the residue
- extractionThe mixture was extracted with dichloromethane (3×100 ml)
- washthe extracts were washed with brine (50 ml)
- dry with materialdried (MgSO4)