反应详情

温度

110 °C

Sodium anthraquinone-1-sulfonate (50.0 g) was combined with POCl3 (31 mL) and a 1:2 (v/v) mixture of sulfolane (100 mL) and acetonitrile (200 mL). The mixture was stirred and heated to 110° C. under a nitrogen atmosphere for 44 hours. The mixture was allowed to cool to room temperature and was then further cooled in a refrigerator. The mixture was filtered and the filtrate was poured onto ice in a beaker and this mixture was stirred for 1 hour. The brown precipitate was filtered, washed with deionized water, dried in air and then further dried overnight in a vacuum oven at 45° C. and less than 1 mmHg pressure to give 12.08 g of the product as a brown solid.

1. temperatureto cool to room temperature
2. temperaturewas then further cooled in a refrigerator
3. filtrationThe mixture was filtered
4. additionthe filtrate was poured onto ice in a beaker
5. stirringthis mixture was stirred for 1 hour
6. filtrationThe brown precipitate was filtered
7. washwashed with deionized water
8. customdried in air
9. customfurther dried overnight in a vacuum oven at 45° C.