反应详情

To a mixture of 3-(2-dimethylamino-ethoxy)-4-trifluoromethyl-phenylamine (0.10 g, 0.4 mmol) in CHCl3 (2.5 mL) was added 4-(3-chloro-2-cyano-phenoxy) benzenesulfonyl chloride (0.13 g, 0.4 mmol) at rt. After stirring at rt for 72 h, the solvent was evaporated and the residue was purified by vacuum filtration through silica gel eluting successively with 4% MeOH in CH2Cl2 and 10% MeOH in CH2Cl2 followed by a mixture of CH2Cl2, MeOH and conc. NH4OH (90:10:1). The solvent was removed from the desired fractions and the residue was recrystallized from a mixture of MeOH and EtOAc to afford the title compound as a white solid; yield 0.01 g (5%): LCMS 540 (M++H).

1. customthe solvent was evaporated
2. filtrationthe residue was purified by vacuum filtration through silica gel eluting successively with 4% MeOH in CH2Cl2 and 10% MeOH in CH2Cl2
3. additionfollowed by a mixture of CH2Cl2, MeOH and conc. NH4OH (90:10:1)
4. customThe solvent was removed from the desired fractions
5. customthe residue was recrystallized from a mixture of MeOH and EtOAc