反应详情

To a stirred solution of methyl 2-(4-methylphenylsulfonamido)acetate (3.10 g, 12.8 mmol) and Cs2CO3 (8.31 g, 25.5 mmol) in DMF (0.1 M) was added MeI (877 μL, 14.1 mmol). The reaction was allowed to stir overnight at rt. The reaction was then diluted with water and repeatedly extracted with CH2Cl2. The combined organic extracts were washed with brine, dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to furnish 6 (2.80 g, 85%): δH (400 MHz, CDCl3) 2.42 (s, 3H, CH3), 2.87 (s, 3H, CH3), 3.66 (s, 3H, CH3), 3.97 (s, 2H, CH2), 7.31 (d, J=8.4 Hz, 2H, CH), 7.69 (d, J=8.4 Hz, 2H, CH); LRMS (ES+) calcd for [C11H15NO4S+H] 258.08. found 258.06 [M+H].

1. extractionrepeatedly extracted with CH2Cl2
2. washThe combined organic extracts were washed with brine
3. dry with materialdried over anhydrous Na2SO4
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure