反应详情

In the same reactor used in Example 2A, there were placed 26.5 g (0.27 mole) of maleic anhydride, 0.7 g of phosphoric acid and 150 ml of mixed xylene. A solution was then added dropwise thereto under reflux of xylene, the solution having been prepared by thermally dissolving 52.8 g (0.1 mole) of 1,4-bis[4(4-aminophenoxy),α,α-dimethylbenzyl)benzene obtained in Example 1A in a mixture of 100 ml of mixed xylene and 50 ml of N,N-dimethylformamide. A dropping time of 5 hours and an aging time of 2 hours were used in order to carry out the reaction. The reaction solution was concentrated to about 1/2 the original amount and then cooled. When a temperature of 80° C. had been reached; 50 g of water was added thereto. Afterward, the solution was slowly cooled with stirring, so that crystals were precipitated. The crystals were then cooled to room temperature, filtered, and washed with cold methanol. 66.5 g of desired crude 1,4-bis[4-(4-maleimidophenoxy)-α, α-dimethylbenzyl]benzene was obtained. Its yield was 96.7%, and its purity according to HLC was 97.5%.

1. additionA solution was then added dropwise
2. customthe solution having been prepared
3. customA dropping time of 5 hours
4. customan aging time of 2 hours
5. customthe reaction
6. concentrationThe reaction solution was concentrated to about 1/2 the original amount
7. temperaturecooled
8. customa temperature of 80° C.
9. addition50 g of water was added
10. temperatureAfterward, the solution was slowly cooled
11. customwere precipitated
12. filtrationfiltered
13. washwashed with cold methanol