反应详情

温度

50 °C

Suberanilic acid (Compound 3, 249.3 g, 1.0 mole) and methanol (0.4-0.5 L) are combined and heated to 45-55° C. The pH is adjusted to ≦2 using hydrochloric acid, and the batch temperature is maintained at 45-55° C. until the reaction is complete. The reaction is quenched with deionized water (0.1-0.2 L). The batch is cooled to 25-30° C. and seeded to induce crystallization, and then cooled to 0-10° C. The batch is filtered, and the cake washed with a 50:50 (v/v) methanol/water solution (0.28-0.34 L) at 0-10° C. The wet cake is dried at a maximum of 46° C. under vacuum to yield methyl suberanilate.

1. temperaturethe batch temperature is maintained at 45-55° C. until the reaction
2. customThe reaction is quenched with deionized water (0.1-0.2 L)
3. temperatureThe batch is cooled to 25-30° C.
4. customcrystallization
5. temperaturecooled to 0-10° C
6. filtrationThe batch is filtered
7. washthe cake washed with a 50:50 (v/v) methanol/water solution (0.28-0.34 L) at 0-10° C
8. customThe wet cake is dried at a maximum of 46° C. under vacuum