反应详情

Methyl 3-amino-4-methylbenzoate (3.18 g), 2-bromo-5-methoxybenzene-1-carbonyl chloride (4.8 g) and triethylamine (5.4 ml) in THF (45 ml) were stirred at room temperature for 2.5 hour and then concentrated. The residue was dissolved in ethyl acetate and washed with 1N HCl, water, brine, dried (magnesium sulfate) and concentrated. The residue was recrystallised from hot ethyl acetate, washed with ether, and air dried to yield methyl 3-[(2-bromo-5-methoxybenzoyl)amino]-4-methylbenzoate as a white solid (5.36 g); NMR Spectrum: (DMSOd6) 2.39 (s, 3H), 3.83 (s, 3H), 3.87 (s, 3H), 7.02 (m, 1H), 7.23 (d, 1H), 7.42 (d, 1H), 7.60 (d, 1H), 7.75 (m, 1H), 8.12 (s, 1H), 10.06 (s, 1H); Mass Spectrum: M+H+ 377.

1. concentrationconcentrated
2. dissolutionThe residue was dissolved in ethyl acetate
3. washwashed with 1N HCl, water, brine
4. dry with materialdried (magnesium sulfate)
5. concentrationconcentrated
6. customThe residue was recrystallised from hot ethyl acetate
7. washwashed with ether, and air
8. customdried