反应详情

A mixture of 3-nitrophthalic acid (35 g) in ethanol (300 ml) containing conc. sulfuric acid (20 ml) was heated under reflux for 24 hours. The solvent was evaporated in vacuo and the residue was poured into cold water (700 ml). The mixture was extracted with ethyl acetate. The organic layer was washed with water and shaken with an aqueous solution of potassium carbonate. The aqueous layer was made acidic with hydrochloric acid and the mixture was extracted with methylene chloride. The organic layer was washed with water, then dried, followed by evaporation of the solvent. The resultant solid (29 g, 74%) was used for the subsequent reaction without purification.

1. temperaturewas heated
2. temperatureunder reflux for 24 hours
3. customThe solvent was evaporated in vacuo
4. additionthe residue was poured into cold water (700 ml)
5. extractionThe mixture was extracted with ethyl acetate
6. washThe organic layer was washed with water
7. extractionthe mixture was extracted with methylene chloride
8. washThe organic layer was washed with water
9. customdried
10. customfollowed by evaporation of the solvent
11. customThe resultant solid (29 g, 74%) was used for the subsequent reaction without purification