反应详情

step 1—To a solution of 58 (150 mg) in DMF (10 mL) cooled to 0° C. was added MeNH2 (0.52 mL, 2.0 M in THF,), HOBt (140 mg) and EDCI (200 mg). The reaction mixture was then stirred overnight at RT then diluted with 1N aq HCl solution and extracted with EtOAc. The organic layer was washed sequentially with water and brine, dried (Na2SO4), filtered and concentrated. The crude residue was purified by SiO2 chromatography eluting with a MeOH/DCM gradient (0 to 10% MeOH) to afford 140 mg of 2-bromo-4-tert-butyl-5-methoxy-N-methyl-benzamide (60) as a white solid.

1. extractionextracted with EtOAc
2. washThe organic layer was washed sequentially with water and brine
3. dry with materialdried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated
6. customThe crude residue was purified by SiO2 chromatography
7. washeluting with a MeOH/DCM gradient (0 to 10% MeOH)