反应详情

温度

100 °C

7.20 g (0.039 mol) of disodium 3,5-diaminophthalate, dissolved in 200 ml of water, are added to a solution of 8.82 g (0.078 mol) of dimethylmaleic anhydride in 80 ml of toluene. This mixture is boiled under reflux for 1 hour. It is then evaporated to dryness in a rotary evaporator, the residue is dissolved, at 90° C., in 100 ml of N,N-dimethylacetamide and 50 ml of water and the solution is rendered acid to Congo Blue with 10% strength hydrochloric acid. After cooling, the slurry-like mixture is filtered and the residue is rinsed with acetone and then dried in vacuo at 80° C. The dry residue is then suspended in 100 ml of acetic anhydride and this mixture is warmed to about 100° C. for 1 hour. It is then evaporated to dryness and the residue is recrystallised from 1,2-dichlorobenzene. 8.9 g (69% of theory) of 3,5-bis-(dimethylmaleimidyl)-phthalic anhydride are obtained; colour: light brownish; melting point 298° C. (decomposition).

1. temperatureunder reflux for 1 hour
2. customIt is then evaporated to dryness in a rotary evaporator
3. dissolutionthe residue is dissolved, at 90° C., in 100 ml of N,N-dimethylacetamide
4. temperatureAfter cooling
5. filtrationthe slurry-like mixture is filtered
6. washthe residue is rinsed with acetone
7. customdried in vacuo at 80° C
8. customIt is then evaporated to dryness
9. customthe residue is recrystallised from 1,2-dichlorobenzene