反应详情

温度

2.5 °C

4-Hydroxy carbazole (60 g) obtained in step 1 was charged into a reactor containing water (90 ml). Epichlorohydrin (64.2 g) and tetrabutyl ammonium bromide (6.3 g) were then charged into the reactor under stirring. 50% Sodium hydroxide solution (78 g) was added slowly in 2-3 hours into the reaction mass at about 30° C. After completion of reaction, ethyl acetate (315 ml) and potable water (315 ml) were charged into the reaction mass. The lower aqueous layer was separated and discarded. The ethyl acetate layer was washed with potable water to obtain neutral pH and dried over anhydrous sodium sulphate. The ethyl acetate is distilled out under vacuum below 55° C. to about 100 ml. The reaction mass was chilled to 0-5° C. and filtered and dried at 50-60° C. to give the title compound (50 g) (64%).

1. additionwere charged into the reaction mass
2. customThe lower aqueous layer was separated
3. washThe ethyl acetate layer was washed with potable water
4. customto obtain neutral pH
5. dry with materialdried over anhydrous sodium sulphate
6. distillationThe ethyl acetate is distilled out under vacuum below 55° C. to about 100 ml
7. filtrationfiltered
8. customdried at 50-60° C.