反应详情

Triethylamine (410 μL, 2.9 mmol) was added to a solution of ethyl 5-(cyclohexylmethyl)piperidine-3-carboxylate (180 mg, 0.71 mmol) and acetyl chloride (120 mg, 1.4 mmol) in CH2Cl2 (10 mL). The reaction was maintained at room temperature for 30 min before being diluted with CH2Cl2 (20 mL) and poured into HCl (1 N, 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 and purification by silica gel chromatography (hexane→80% EtOAc/hexane) provided the title compound as a yellow oil. MS m/z: 296.1 (M+1).

1. customThe layers were separated
2. extractionthe aqueous layer was extracted with CH2Cl2 (3×20 mL)
3. washThe combined organic layers were sequentially washed with H2O (10 mL) and brine
4. dry with materialbefore being dried over Na2SO4
5. concentrationConcentration
6. customunder reduced pressure and purification by silica gel chromatography (hexane→80% EtOAc/hexane)