反应详情

To 4-bromo-2-fluoro-1-methylsulfonyl-benzene (2 g, 7.9 mmol) in DMF (15 mL) is added 2-methanesulfonyl-ethanol (1.47 g, 11.85 mmol). Sodium hydride (948.16 mg, 23.71 mmol) is added in portions at 0° C. The reaction mixture is allowed to come to r.t. and is added dropwise into cooled aq. hydrochloric acid. The aq. layer is extracted with ethyl acetate. The organic layer is dried over MgSO4, filtered and concentrated. The crude residue is purified by reversed phase HPLC. Yield 86%, m/z 251/253[M+H]+, rt 0.42 min, LC-MS Method X018_S01.

1. customto come to r.t.
2. additionis added dropwise
3. extractionThe aq. layer is extracted with ethyl acetate
4. dry with materialThe organic layer is dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe crude residue is purified by reversed phase HPLC
8. customYield 86%, m/z 251/253[M+H]+, rt 0.42 min, LC-MS Method X018_S01