反应详情

To a solution of 0.70 g (1.52 mmol) of methyl 2-[(2-diacetylaminobenzyl)-(4-methoxybenzenesulfonyl)amino]acrylate in 5 ml of anhydrous methanol was added 0.332 g (3.95 mmol) of anhydrous sodium bicarbonate. The mixture was stirred at room temperature overnight and the solvent removed under vacuum. To the residue was added ethyl acetate and H2O. The organic layer was separated, washed with brine and dried with Na2SO4. The solvent was removed and the residue dried under vacuum to give 0.59 g of white crystals, m.p. 150-155° C. Anal. for C20H22N2O6S: Calc'd: C,57.4; H,5.3; N,6.7; S,7.7; Found: C,56.6; H,5.2; N,6.5; S,7.5; Mass spectrum (ES) 419.9 (M+H).

1. customthe solvent removed under vacuum
2. additionTo the residue was added ethyl acetate and H2O
3. customThe organic layer was separated
4. washwashed with brine
5. dry with materialdried with Na2SO4
6. customThe solvent was removed
7. customthe residue dried under vacuum