반응 #1841

반응 방정식

phenol

potassium carbonate

5-fluoro-2-nitrotoluene

→

2-Nitro-5-phenoxytoluene

용매

N,N-dimethylacetamide

반응 조건

후처리

1. 1
   workup.STIRRINGthe mixture was stirred at 70°-80° C. for 30 minutes
2. 2
   온도the mixture was heated at 135°-140° C. for 2 hours
3. 3
   온도after cooling
4. 4
   농축concentrated in vacuo
5. 5
   workup.ADDITIONthe residue was introduced into ice
6. 6
   여과the crystalline product was filtered off with suction
7. 7
   세척washed with water
8. 8
   기타dried

실험 절차

14.1 g (150 mmol) of phenol were dissolved in 120 ml of anhydrous N,N-dimethylacetamide, while stirring, 20.6 g (150 mmol) of finely powdered potassium carbonate were added and the mixture was stirred at 70°-80° C. for 30 minutes. After cooling to 20° C., 23.25 g (18.3 ml, 150 mmol) of 5-fluoro-2-nitrotoluene were added dropwise, the mixture was heated at 135°-140° C. for 2 hours and, after cooling, concentrated in vacuo, the residue was introduced into ice and the crystalline product was filtered off with suction, washed with water and dried, 30 g, melting point 43°-46° C.

출처