反应详情

1-Benzyl-3-(trifluoromethyl)piperazine (0.74 g, 3.0 mmol; Intermediate 44) was dissolved in acetic acid (70 mL) and water (5 mL). Pd, 5% on carbon, (0.074 g) was added and =hydrogenation was performed at 3 bar and 70° C. overnight. The reaction mixture was filtered through Celite and the pad was rinsed with water (5 mL). Solvents were removed in vacuo, toluene (20 mL) added to the residue, followed by re-concentration in vacuo to remove residual water. The desired product sublimated on the evaporator and 0.15 g (32%) was collected as a white powder. 1H NMR (270 MHz, methanol-d4) δ ppm 2.67-2.87 (m, 3H) 2.91-3.05 (m, 2H) 3.12-3.21 (m, 1H). MS (ESI+) m/z 155. *Previously described in Rec. Trav. Chim. Pays-Bas 1995, 114, 97-102.

1. customwas performed at 3 bar and 70° C. overnight
2. filtrationThe reaction mixture was filtered through Celite
3. washthe pad was rinsed with water (5 mL)
4. customSolvents were removed in vacuo, toluene (20 mL)
5. additionadded to the residue
6. concentrationfollowed by re-concentration in vacuo
7. customto remove residual water
8. customThe desired product sublimated on the evaporator and 0.15 g (32%)
9. customwas collected as a white powder