反应详情

Sodium hydride (1.68 g×60% ) was added to a stirred solution of methanesulfonamide (2.0 g) in dry tetrahydrofuran (20 ml) at room temperature. The resulting solution was stirred at room temperature for 1 hour, as which time it was treated with a solution of bromoacetyl bromide (4.2 g) in dry tetrahydrofuran (10 ml). After 1 hour the solvent was removed under reduced pressure and the residue taken up in water and acidified to pH3. The acidic solution was extracted into ethyl acetate, dried (MgSO4), filtered and the solvent removed under reduced pressure. Recrystallisation from isopropanol afforded the product as white needles: mp 112°-114° C.

1. customAfter 1 hour the solvent was removed under reduced pressure
2. extractionThe acidic solution was extracted into ethyl acetate
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. customthe solvent removed under reduced pressure
6. customRecrystallisation from isopropanol