반응 #56523

반응 방정식

2-chloro-5-nitro-benzotrifluoride

potassium hydroxide

hydrochloric acid

→

4-nitro-2-trifluoromethylphenol

용매

methanol

반응 조건

후처리

1. 1
   기타being kept at a maximum of 40° C.
2. 2
   온도by cooling
3. 3
   workup.ADDITIONAbout 30 minutes after the addition
4. 4
   온도cooled
5. 5
   추출The mixture is extracted several times with 300 ml of methylene chloride each time
6. 6
   건조the organic phase is dried with sodium sulphate
7. 7
   기타About 413 g of crude product, melting point: 90°-95° C., are obtained with a purity of about 95%
8. 8
   기타After recrystallisation
9. 9
   workup.DISTILLATIONfrom toluene, or distillation under 0.5 mm

실험 절차

450 g of 2-chloro-5-nitro-benzotrifluoride in 1,250 ml of methanol and 35 g of tetraethylammonium chloride are initially introduced. 1,000 g of an aqueous, 50% strength potassium hydroxide solution are then added dropwise (1 hour), the temperature being kept at a maximum of 40° C. by cooling. About 30 minutes after the addition has ended, the mixture is heated to 80° C. for 6 hours, cooled and rendered acid with concentrated hydrochloric acid. The mixture is extracted several times with 300 ml of methylene chloride each time, and the organic phase is dried with sodium sulphate and freed from the solvent under reduced pressure. About 413 g of crude product, melting point: 90°-95° C., are obtained with a purity of about 95% according to analysis by gas chromatography. After recrystallisation from toluene, or distillation under 0.5 mm, pure 4-nitro-2-trifluoromethylphenol is obtained, melting point: 134° C.

출처