反应详情

A mixture of 1-methyl-2-oxo-3-piperidinyl methanesulfonate (1.7 g., 0.008 mole) and potassium thioacetate (1.39 g., 0.012 mole) in 80 ml. acetone was refluxed under nitrogen for 20 hours. The reaction mixture was concentrated in vacuo and the residue was dissolved in 50 ml. ethyl acetate and 50 ml. water. The ethyl acetate layer was washed with 50 ml. water and 50 ml saturated aqueous sodium chloride solution, dried over anhydrous sodium acetate and concentrated in vacuo. The residue was chromatographed on silica gel eluting with ethyl acetate to yield 600 mg (40% yield) of the title compound. NMR (CDCl3): 1.7-2.5 (c) and 2.38 (s) (total 7H); 3.0 (s, 3H); 3.36 (m, 2H); and 4.2 (m, 1H)ppm.

1. concentrationThe reaction mixture was concentrated in vacuo
2. dissolutionthe residue was dissolved in 50 ml
3. washThe ethyl acetate layer was washed with 50 ml
4. dry with materialwater and 50 ml saturated aqueous sodium chloride solution, dried over anhydrous sodium acetate
5. concentrationconcentrated in vacuo
6. customThe residue was chromatographed on silica gel eluting with ethyl acetate