反应详情

To a solution of EXAMPLE 296C (0.175 g) in tetrahydrofuran (5 ml) was added sodium hydride (0.209 g) and the reaction stirred at room temperature for 15 minutes. 3-Chloro-4-fluorobenzenesulfonamide (0.273 g) was added and the reaction stirred for 3 hours. To the thick suspension was added tetrahydrofuran (2 ml) and N,N-dimethylformamide ml). The reaction was stirred for 3 hours at 60° C. then poured into dichloromethane (50 ml) and 1N aqueous HCl (50 ml). The organic layer was washed with brine (35 ml) dried over magnesium sulfate, filtered, and concentrated. Silica gel chromatography (Reveleris 40 g) eluting with a gradient of 10-100% ethyl acetate, hexanes over 30 minutes (flow=40 ml/minute) gave the title compound.

1. stirringthe reaction stirred for 3 hours
2. stirringThe reaction was stirred for 3 hours at 60° C.
3. washThe organic layer was washed with brine (35 ml)
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. washSilica gel chromatography (Reveleris 40 g) eluting with a gradient of 10-100% ethyl acetate, hexanes over 30 minutes (flow=40 ml/minute)