反应详情

To a mixture of 10.0 g (66.0 mmol) of 3-methylanthranilic acid in 60 mL of 1,4-dioxane was slowly added 100 mL (193 mmol) of a 1.93 molar solution of phosgene in toluene, at room temperature. The mixture was stirred overnight. The mixture was concentrated in vacuo to yield a residue which was triturated with ethyl acetate-hexane (1:4), filtered, washed with hexane and dried to afford 11.66 g (99.5%) of the 3-methylisatoic anhydride as an off white solid. MS (Cl mode) m/z 160 (M-18, 100%), 178 (M+H, 90%).

1. customat room temperature
2. concentrationThe mixture was concentrated in vacuo
3. customto yield a residue which
4. customwas triturated with ethyl acetate-hexane (1:4)
5. filtrationfiltered
6. washwashed with hexane
7. customdried