反应详情

温度

165 °C

To 4-aminobenzoic acid (800 g, 5.83 mol) is added dimethylacetamide (2.5 l), toluene (1 l), and slowly with stirring bicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic anhydride (956 g, 5.83 mol). After the addition the mixture is stirred for 1 hour, raised to 140° C. with removal of water (100 ml) azeotropically and then raised to 165° C. to remove the toluene. The mixture is cooled and the product precipitated into water (3 l). Filtration, washing with water, drying in an oven at 80° C. and recrystallisation from ethanol yields a white crystalline solid (1.56 kg, 94%). M.p.: 224°-228° C.

1. additionAfter the addition the mixture
2. customto remove the toluene
3. temperatureThe mixture is cooled
4. customthe product precipitated into water (3 l)
5. filtrationFiltration
6. washwashing with water
7. customdrying in an oven at 80° C.
8. customrecrystallisation from ethanol