반응 #56524

반응 방정식

hydrochloric acid

4-chloro-3-nitro-benzotrifluoride

benzyldodecyldimethylammonium chloride

potassium hydroxide

→

2-nitro-4-trifluoromethylphenol

수율 92.0%

용매

ethylene glycol monomethyl ether

반응 조건

후처리

1. 1
   workup.ADDITIONare added dropwise in the course of about 30 minutes, up to a temperature of 65° C
2. 2
   온도subsequently cooled
3. 3
   기타The organic phase is separated off
4. 4
   세척washed with 20 ml of dilute hydrochloric acid
5. 5
   기타the organic phase is again separated off
6. 6
   건조dried with sodium sulphate

실험 절차

45 g of 4-chloro-3-nitro-benzotrifluoride and 10 ml of 50% strength aqueous benzyldodecyldimethylammonium chloride are initially introduced into 150 ml of ethylene glycol monomethyl ether, and 100 g of 50% strength potassium hydroxide solution are added dropwise in the course of about 30 minutes, up to a temperature of 65° C. The mixture is then stirred at 65° C. for 6 hours and subsequently cooled and rendered acid with concentrated hydrochloric acid, and about 500 ml of distillate are driven over with steam. The organic phase is separated off and washed with 20 ml of dilute hydrochloric acid, and the organic phase is again separated off and dried with sodium sulphate. 38 g of 2-nitro-4-trifluoromethylphenol are obtained, which corresponds to a yield of 92% of theory.

출처