تفاعل #56524

معادلة التفاعل

hydrochloric acid

4-chloro-3-nitro-benzotrifluoride

benzyldodecyldimethylammonium chloride

potassium hydroxide

→

2-nitro-4-trifluoromethylphenol

المردود 92.0%

المذيبات

ethylene glycol monomethyl ether

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONare added dropwise in the course of about 30 minutes, up to a temperature of 65° C
2. 2
   درجة الحرارةsubsequently cooled
3. 3
   أخرىThe organic phase is separated off
4. 4
   غسيلwashed with 20 ml of dilute hydrochloric acid
5. 5
   أخرىthe organic phase is again separated off
6. 6
   تجفيفdried with sodium sulphate

الإجراء التجريبي

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.

المصدر