反应详情

温度

0 °C

Triethylamine (340 mL, 2.4 mmol) was added to a solution of ethyl 5-(cyclohexylmethyl)piperidine-3-carboxylate (155 mg, 0.60 mmol) and methanesulfonyl chloride (75 mL, 0.90 mmol) in CH2Cl2 (6 mL) cooled to 0° C. The reaction was maintained at this temperature for 15 min at which point the whole was allowed to warm to RT and stir for an additional 3 h. The reaction was diluted with CH2Cl2 (20 mL) and poured into HCl (1N, 20 mL). The layers were separated and the aqueous layer was extracted with CH2Cl2 (3×20 mL). The combined organic layers were sequentially washed with H2O (10 mL) and brine before being dried over Na2SO4. Concentration under reduced pressure provided the title compound. MS m/z: 332.1 (M+1).

1. temperatureThe reaction was maintained at this temperature for 15 min at which point the whole
2. temperatureto warm to RT
3. customThe layers were separated
4. extractionthe aqueous layer was extracted with CH2Cl2 (3×20 mL)
5. washThe combined organic layers were sequentially washed with H2O (10 mL) and brine
6. dry with materialbefore being dried over Na2SO4
7. concentrationConcentration under reduced pressure