反应详情

A cocktail containing 40% trifluoroacetic acid, 1% trifluoromethanesulfonic acid in CH2Cl2 (20 ml) was added to 4-chloro-N-[(R)-1-(2,4-dimethoxy-benzyl)-5,5-difluoro-2-oxo-azepan-3-yl]-benzenesulfonamide (0.5 g, 1.0 mmol). After 30 min the reaction mixture was concentrated and the residue was dissolved in ethyl acetate and washed with water, NaHCO3 solution, 1 M KHSO4 solution, brine, dried (MgSO4.2H2O), filtered, concentrated under reduce pressure and purified over silica gel (CH2Cl2/MeOH 95:5 v/v): white solid 0.74 g (78%);

1. concentrationAfter 30 min the reaction mixture was concentrated
2. dissolutionthe residue was dissolved in ethyl acetate
3. washwashed with water, NaHCO3 solution, 1 M KHSO4 solution, brine
4. dry with materialdried (MgSO4.2H2O)
5. filtrationfiltered
6. concentrationconcentrated
7. custompurified over silica gel (CH2Cl2/MeOH 95:5 v/v)