反应详情

温度

23 °C

A mixture of (R)-5-(5-bromo-2-fluoro-phenyl)-4-(2,4-dimethoxy-benzyl)-5-methyl-1,1-dioxo-1λ6-thiomorpholin-3-one (251 mg, 516 μmol, Eq: 1.00) and trifluoroacetic acid (5.88 g, 3.98 ml, 51.6 mmol, Eq: 100) was stirred at 23° C. for 16 hours. Poured into 1 M Na2CO3-sol. and extracted twice with ethyl acetate. The combined organic layers were dried over Na2SO4, filtered and evaporated. The residue was chromatographed on 5 g silica gel with dichloromethane/ethyl acetate 9:1 to give (R)-5-(5-bromo-2-fluoro-phenyl)-5-methyl-1,1-dioxo-1λ6-thiomorpholin-3-one (116 mg, 345 μmol, 66.9% yield) as a white solid. MS (ISN): m/z=334.0 [M−H]− and 336.0 [M+2−H]−.

1. extractionand extracted twice with ethyl acetate
2. dry with materialThe combined organic layers were dried over Na2SO4
3. filtrationfiltered
4. customevaporated
5. customThe residue was chromatographed on 5 g silica gel with dichloromethane/ethyl acetate 9:1