反应详情

Hydrogen chloride was passed into a solution of 3,4-dimethoxyanthranilic acid (100 g., 0.51 mole) in 1.5 liters methanol for 40 minutes. The reaction mixture was refluxed for 4 days while introducing hydrogen chloride gas intermittently. The solvent was removed in vacuo, and the residual white solid was dissolved in 500 ml. water, cooled and basified to pH 10 with sodium hydroxide solution. After cooling for an additional hour, the cream color product (87.0 g., 82% yield) was filtered. Recrystallization from methanol furnished pure product, M.P. 66°-67° C.

1. temperatureThe reaction mixture was refluxed for 4 days
2. customThe solvent was removed in vacuo
3. dissolutionthe residual white solid was dissolved in 500 ml
4. temperaturewater, cooled
5. temperatureAfter cooling for an additional hour
6. filtrationthe cream color product (87.0 g., 82% yield) was filtered
7. customRecrystallization from methanol furnished pure product, M.P. 66°-67° C.