反应详情

A solution of 2-(4-chloro-3-fluoro-phenyl)-1-(2-phenyl-piperidin-1-yl)-ethanone (0.25 g, 0.75 mmol), N,N-diethyl-2-phenyl-2-piperazin-1-yl-acetamide (0.23 g, 0.82 mmol), Pd2(dba)3 (0.01 g, 0.0075 mmol), XPhos (0.01 g, 0.015 mmol), and sodium t-butoxide (0.11 g, 1.05 mmol) in toluene (2 mL) was irradiated by microwave at 120° C. for 20 min. The solution was allowed to cool, filtered through diatomaceous earth, washing with DCM (10 mL). The filtrate was concentrated and the residue was purified by SiO2 column chromatography (2 M NH3 in MeOH:DCM) to provide the title compound (0.07 g, 16%). MS: 571.7. 1H NMR (CDCl3): 7.48-7.46 (m, 2H), 7.38-7.35 (m, 4H), 7.28-7.23 (m, 2H), 7.19-7.15 (m, 4H), 6.90-6.89 (m, 2H), 3.70 (bs, 2H), 3.49-3.40 (m, 6H), 3.31-3.12 (m, 8H), 2.70-2.69 (m, 4H), 1.60-1.59 (m, 3H), 1.10-1.04 (m, 6H).

1. temperatureto cool
2. filtrationfiltered through diatomaceous earth
3. washwashing with DCM (10 mL)
4. concentrationThe filtrate was concentrated
5. customthe residue was purified by SiO2 column chromatography (2 M NH3 in MeOH:DCM)