反应详情

To a liquid mixture consisting of 24 parts of tetrabromoterephthalic acid and 60 parts of chloroform, were dropped with stirring 20 parts of allyl chloroacetate. Thereafter, 13 parts of triethylamine were added dropwise while cooling the resulting mixture at 15°-20° C. The mixture was heated until chloroform started to reflux. At the same temperature, the mixture was maintained for 8 hours. After allowing the liquid reaction mixture to cool, it was poured in a separation funnel and washed first with dilute hydrochloric acid and then with water. The organic layer was concentrated under reduced pressures and the resulting white solid was recrystallized from ethyl acetate, thereby obtaining 25 parts of bis(allyloxycarbonylmethyl) tetrabromoterephthalate (hereinafter called "Compound E") as white irregular crystals. (m.p. 146°-148° C.).

1. additionwere dropped
2. temperaturewhile cooling the resulting mixture at 15°-20° C
3. temperatureto reflux
4. temperatureAt the same temperature, the mixture was maintained for 8 hours
5. customthe liquid reaction mixture
6. temperatureto cool
7. additionit was poured in a separation funnel
8. washwashed first with dilute hydrochloric acid
9. concentrationThe organic layer was concentrated under reduced pressures
10. customthe resulting white solid was recrystallized from ethyl acetate