反应详情

温度

23 °C

To a solution of (R)-5-(5-bromo-2-fluorophenyl)-4-(2,4-dimethoxybenzyl)-5-methylthiomorpholin-3-one (2.95 g, 6.49 mmol, Eq: 1.00) in methanol (100 ml) was added at 23° C. Oxone® (7.98 g, 13.0 mmol, Eq: 2.00). The reaction mixture was stirred at 23° C. for 16 hours. The reaction mixture was carefully quenched by addition of water at 0° C., then 10 ml of a diluted NaHSO3-solution, sat. NaHCO3-solution and ethyl acetate were added. Vigorous stirring was continued for 10 min. The organic layer was separated and washed with water, then dried over Na2SO4, filtered and evaporated to give a yellow oil which was chromatographed on 20 g silica gel with 0-50% ethyl acetate in heptane to give (R)-5-(5-bromo-2-fluoro-phenyl)-4-(2,4-dimethoxy-benzyl)-5-methyl-1,1-dioxo-1λ6-thiomorpholin-3-one (3 g, 6.17 mmol, 95.0% yield) as a white foam. MS (ISP): m/z=486.2 [M+H]+ and 488.1 [M+2+H]+.

1. customThe reaction mixture was carefully quenched by addition of water at 0° C.
2. addition10 ml of a diluted NaHSO3-solution, sat. NaHCO3-solution and ethyl acetate were added
3. stirringVigorous stirring
4. waitwas continued for 10 min
5. customThe organic layer was separated
6. washwashed with water
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. customevaporated
10. customto give a yellow oil which
11. customwas chromatographed on 20 g silica gel with 0-50% ethyl acetate in heptane