反应详情

A mixture of 5-bromo-4-chloro-2-fluoro-N-methyl-N-o-tolyl-benzamide (2.5 g, 7.0 mmol) was heated in MeONa/MeOH (20 mL, 25%) at 55° C. for 12 hrs, then was concentrated and partitioned between DCM and water. The organic layer was then separated, washed with 3N HCl, sat NaHCO3 and brine, dried over MgSO4, and concentrated. Purification by silica gel column chromatography eluting with ethyl acetate in hexanes (1/4) gave 5-bromo-4-chloro-2-methoxy-N-methyl-N-o-tolyl-benzamide (2.75 g). MS: 367.8 (M+H)+; tR=2.51 min (method 1).

1. concentrationwas concentrated
2. custompartitioned between DCM and water
3. customThe organic layer was then separated
4. washwashed with 3N HCl
5. dry with materialdried over MgSO4
6. concentrationconcentrated
7. customPurification by silica gel column chromatography
8. washeluting with ethyl acetate in hexanes (1/4)