反应详情

温度

75 °C

NaH (55% dispersion in mineral oil, 36 mg, 0.82 mmol) was added portionwise at RT to a solution of 3-methyl-4-(3-trifluoromethoxy-phenyl)-piperazin-2-one (150 mg, 0.55 mmol) in DMA (3 mL), then after 1 h a solution of 1-(3-chloropropyl)-piperidine in toluene [prepared from commercially available 1-(3-chloropropyl)-piperidine hydrochloride (542 mg, 2.74 mmol) by partitioning between toluene (4 ml) and 1 M aq. sodium hydroxide solution (4 ml) and drying of the organic layer with MgSO4] was added. The reaction mixture was heated at 75° C. for 1 h, then partitioned between sat. aq. NaHCO3 solution and CH2Cl2. The organic layer was dried (MgSO4), filtered, and evaporated. Chromatography (IST Isolute® Flash NH2; EtOAc) afforded the title compound (184 mg, 84%). Light yellow oil, MS: 400.3 (M+H)+.

1. customby partitioning between toluene (4 ml) and 1 M aq. sodium hydroxide solution (4 ml)
2. dry with materialdrying of the organic layer with MgSO4]
3. additionwas added
4. custompartitioned between sat. aq. NaHCO3 solution and CH2Cl2
5. dry with materialThe organic layer was dried (MgSO4)
6. filtrationfiltered
7. customevaporated