反应详情

tert-Butyl 4-(propan-2-ylsulfanyl)piperidine-1-carboxylate (prepared in an analogous manner to Intermediate 245, 0.160 g, 0.62 mmol) was dissolved in DCM (3 mL) and cooled to 0 C. m-Chloroperbenzoic acid (0.138 g, 0.62 mmol) was added, the mixture was warmed to room temperature and stirred for 17 h. Further m-chloroperbenzoic acid (0.040 g, 0.18 mmol) was added and the mixture was stirred at room temperature for 3 h. The mixture was then diluted with DCM (10 mL) and washed with saturated aq. sodium thiosulfate (10 mL). The organic layer was separated and purified by FCC, eluting with 50-100% EtOAc in heptane followed by 10% MeOH in EtOAc to afford the title compound as a colourless oil (0.124 g, 73%). Method C HPLC-MS: MH+ requires m/z=276 Found: m/z=298 (M+Na), Rt=1.14 min (100%).

1. temperaturecooled to 0 C
2. stirringthe mixture was stirred at room temperature for 3 h
3. washwashed with saturated aq. sodium thiosulfate (10 mL)
4. customThe organic layer was separated
5. custompurified by FCC
6. washeluting with 50-100% EtOAc in heptane