反応 #43889

反応方程式

Sodium anthraquinone-1-sulfonate

POCl3

sulfolane

→

product

1-Chlorosulfonylanthraquinone

溶媒

acetonitrile

反応条件

後処理

1. 1
   温度to cool to room temperature
2. 2
   温度was then further cooled in a refrigerator
3. 3
   ろ過The 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
   ろ過The brown precipitate was filtered
7. 7
   洗浄washed with deionized water
8. 8
   その他dried in air
9. 9
   その他further dried overnight in a vacuum oven at 45° C.

実験手順

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.

出典