Reaktion #573062

Reaktionsgleichung

2,3-dichloroanisole

chlorosulfonic acid

→

2,3-dichloro-4-methoxybenzenesulfonyl chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeof 30 minutes
2. 2
   workup.ADDITIONThe reaction is mildly exothermic and at the end of the addition
3. 3
   Sonstigea clear solution is formed
4. 4
   Sonstigequenched with 200 g of crushed ice
5. 5
   FiltrationThe solid is filtered
6. 6
   Sonstigeair-dried
7. 7
   Sonstigerecrystallized from ether-pentane

Vorschrift

To 5.31 g of 2,3-dichloroanisole is slowly added 10 ml of chlorosulfonic acid over a period of 30 minutes. The reaction is mildly exothermic and at the end of the addition, a clear solution is formed. The yellowish solution is stirred at room temperature for 1 additional hour and quenched with 200 g of crushed ice. The solid is filtered, air-dried and recrystallized from ether-pentane to give 6.9 g of 2,3-dichloro-4-methoxybenzenesulfonyl chloride as off-white prisms, mp 93°-95°.

Quelle