Reacción #43889

Ecuación de reacción

Sodium anthraquinone-1-sulfonate

POCl3

sulfolane

→

product

1-Chlorosulfonylanthraquinone

Disolventes

acetonitrile

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturato cool to room temperature
2. 2
   Temperaturawas then further cooled in a refrigerator
3. 3
   FiltraciónThe mixture was filtered
4. 4
   workup.ADDITIONthe filtrate was poured onto ice in a beaker
5. 5
   workup.STIRRINGthis mixture was stirred for 1 hour
6. 6
   FiltraciónThe brown precipitate was filtered
7. 7
   Lavadowashed with deionized water
8. 8
   Otrodried in air
9. 9
   Otrofurther dried overnight in a vacuum oven at 45° C.

Procedimiento

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.

Fuente