反应详情

Combine (S)-1,4-dibenzyl-2-(2-(3-methoxy-phenyl)-ethyl)-piperazine (2.15 g, 5.37 mmol), ammonium formate (1.69 g, 26.84 mmol), 5% Pd/C (259.7 mg), and ethanol (100 mL). Stir and heat the mixture at reflux. After 3 hours, cool to ambient temperature and remove the catalyst by vacuum filtration through celite. Reduce the filtrate to residue and purify it on silica gel using dichloromethane/7N ammonia in methanol (90:10) to give (1.11 g, 94%) of the title compound as a white solid: mp 53–57° C.; mass spectrum (ion spray): m/z=221.1 (M+1); Analysis for C13H20N2O: calcd: C, 70.87; H, 9.15; N, 12.72; found: C, 70.52; H, 9.06; N, 12.74.

1. temperatureheat the mixture
2. temperatureat reflux
3. customremove the catalyst
4. filtrationby vacuum filtration through celite
5. custompurify it on silica gel