反应详情

温度

75 °C

To a solution of 3-(5,5-dimethyl-1,3-dioxan-2-yl)-1-(4-fluorophenyl)propan-1-one (Step 4) (1.68 g, 6.3 mmol) in dimethylformamide (75 ml), methanesulfinic acid sodium salt (2.9 g, 28.4 mmol) was added. The reaction mixture was heated at 120-30° C. for 72 hours. After cooling, the solvent was removed under reduced pressure and the reaction mixture was diluted with water. The material was extracted with methylene chloride and washed with brine. After drying (MgSO4), filtration and concentration, the crude solid (2.78 g) was purified by chromatography (silica gel, hexane/ethyl acetate, 6/4) to give the sulfone (1.62 g, 79%) as a white solid: mp (DSC) 104° C. Anal Calc'd. for C16H22SO5 : C, 58.88; H, 6.79; S, 9.82. Found: C, 58.76; H, 7.01; S, 10.21.

1. temperatureAfter cooling
2. customthe solvent was removed under reduced pressure
3. additionthe reaction mixture was diluted with water
4. extractionThe material was extracted with methylene chloride
5. washwashed with brine
6. customAfter drying
7. filtration(MgSO4), filtration and concentration
8. customthe crude solid (2.78 g) was purified by chromatography (silica gel, hexane/ethyl acetate, 6/4)