反应详情

温度

10 °C

Into a 2 liter three-necked round bottom flask, equipped with a mechanical stirrer and a thermometer, containing 77 g 3-[(2-aminophenyl)thio]-2-n-octyloxy-7H-benzo[de]anthracene-7-one (0.16M), placed into an ice bath, was added 1100 ml of DMF. The mixture was cooled to 10° C. while stirring. 35% Hydrochloric acid (247 ml) was added portionwise, ensuring that the reaction temperature did not exceed 20° C. After the HCl addition was complete, the reaction was cooled to 0° C. and a solution of 14.0 g (0.2M) NaNO2 in 78 ml of H2O was added portionwise, making sure that the reaction temperature did not rise above 5° C. The reaction mixture was held at 5° C. for an additional 1 hour after the completion of the sodium nitrite addition. Then, during the addition of 5.2 g copper sulfate catalyst, the reaction was heated, and at 15° C., nitrogen bubbles began to evolve. The reaction mass was held at 100° C. for 1.5 hours, cooled and the red colored precipitate was filtered and washed with water, then ethanol. The yield=66.89 g (90%); Tm=205-208° C.

1. customInto a 2 liter three-necked round bottom flask, equipped with a mechanical stirrer
2. customplaced into an ice bath
3. customdid not exceed 20° C
4. temperaturethe reaction was cooled to 0° C.
5. customdid not rise above 5° C
6. temperaturethe reaction was heated
7. customat 15° C.
8. waitThe reaction mass was held at 100° C. for 1.5 hours
9. temperaturecooled
10. filtrationthe red colored precipitate was filtered
11. washwashed with water
12. customTm=205-208° C.