반응 #344408

반응 방정식

nitric acid

sulphuric acid

5,6-dichloro-2,2-difluorobenzo[1.3]dioxole

→

5,6-dichloro-4-nitro-2,2-difluoro-benzo(1.3)dioxole

수율 89.0%

반응 조건

후처리

1. 1
   workup.ADDITIONis added dropwise at 5° to 10° C. (internal temperature)
2. 2
   추출extracted with ether
3. 3
   기타the extract is dried
4. 4
   농축concentrated

실험 절차

A precooled mixture of 140 ml of 100% strength nitric acid and 200 ml of 100% strength sulphuric acid is added dropwise at 5° to 10° C. (internal temperature) with good stirring to 219 g (0.96 mol) of 5,6-dichloro-2,2-difluorobenzo[1.3]dioxole. The reaction mixture is then subsequently stirred at room temperature for 6 h. It is added to ice-water and extracted with ether, and the extract is dried and concentrated. 233 g (89% of theory) of 5,6-dichloro-4-nitro-2,2-difluoro-benzo(1.3)dioxole having a melting point of 29°-30° C. are obtained.

출처