反应详情

温度

140 °C

A mixture of 172 mg (0.715 mmol) 1-(5-chloro-2-nitro-phenyl)-piperidine (as prepared in Example 4, step (a)) and 360 μL (3.58 mmol) of thiomorpholine were heated with stirring under Ar at 140° C. for 40 h. After cooling to RT, the mixture was poured into water (50 mL) and extracted with EtOAc (2×20 mL). The combined extracts were washed with water (3×50 mL) and brine (50 mL) and then dried (Na2SO4). Concentration and chromatography on a 10-g silica SPE column with 60% dichloromethane-hexane afforded 145 mg (66%) of the title compound as a yellow resin: Mass spectrum (ESI, m/z): Calcd. for C15H21N3O2S, 308.1 (M+H), found 308.1.

1. temperaturewere heated
2. temperatureAfter cooling to RT
3. extractionextracted with EtOAc (2×20 mL)
4. washThe combined extracts were washed with water (3×50 mL) and brine (50 mL)
5. dry with materialdried (Na2SO4)
6. concentrationConcentration and chromatography on a 10-g silica SPE column with 60% dichloromethane-hexane