反応 #56524

反応方程式

hydrochloric acid

4-chloro-3-nitro-benzotrifluoride

benzyldodecyldimethylammonium chloride

potassium hydroxide

→

2-nitro-4-trifluoromethylphenol

収率 92.0%

溶媒

ethylene glycol monomethyl ether

反応条件

後処理

1. 1
   workup.ADDITIONare added dropwise in the course of about 30 minutes, up to a temperature of 65° C
2. 2
   温度subsequently cooled
3. 3
   その他The organic phase is separated off
4. 4
   洗浄washed with 20 ml of dilute hydrochloric acid
5. 5
   その他the organic phase is again separated off
6. 6
   乾燥dried with sodium sulphate

実験手順

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.

出典