Reaktion #43889

Reaktionsgleichung

Sodium anthraquinone-1-sulfonate

POCl3

sulfolane

→

product

1-Chlorosulfonylanthraquinone

Lösungsmittel

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturto cool to room temperature
2. 2
   Temperaturwas then further cooled in a refrigerator
3. 3
   FiltrationThe 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
   FiltrationThe brown precipitate was filtered
7. 7
   Waschenwashed with deionized water
8. 8
   Sonstigedried in air
9. 9
   Sonstigefurther dried overnight in a vacuum oven at 45° C.

Vorschrift

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.

Quelle