反应详情

N-{2-Fluoro-5-[(1Z)-N-hydroxyethanimidoyl]phenyl}methanesulfonamide (Method 62, 200 mg, 812 μmol) was dissolved in 15 ml THF, to which was added Raney nickel 2800 slurry in water (200 μl). The mixture was charged with nitrogen and stirred over 1 atm of hydrogen. After 1 hour, MeOH (4 ml) was added and the reaction mixture was stirred overnight. The following morning the solution was filtered through celite, and the cake washed with MeOH, and the organic layer was concentrated to a yellow solid which was dried under high vacuum (181 mg, 96%). 1H NMR: 1.26 (d, 3H, CH3), 2.92 (s, 3H, SO2Me), 3.33 (HOD), 4.04 (q, 1H, CH), 5.70 (br, 2H, NH2), 7.06-7.16 (m, 2H, Ar), 7.35 (m, 1H, Ar). LC/MS: 0.79 min, 231.08 (M−H)−.

1. additionThe mixture was charged with nitrogen
2. filtrationThe following morning the solution was filtered through celite
3. washthe cake washed with MeOH
4. concentrationthe organic layer was concentrated to a yellow solid which
5. customwas dried under high vacuum (181 mg, 96%)
6. custom0.79 min, 231.08 (M−H)−