反応 #1841

反応方程式

phenol

potassium carbonate

5-fluoro-2-nitrotoluene

→

2-Nitro-5-phenoxytoluene

溶媒

N,N-dimethylacetamide

反応条件

後処理

1. 1
   workup.STIRRINGthe mixture was stirred at 70°-80° C. for 30 minutes
2. 2
   温度the mixture was heated at 135°-140° C. for 2 hours
3. 3
   温度after cooling
4. 4
   濃縮concentrated in vacuo
5. 5
   workup.ADDITIONthe residue was introduced into ice
6. 6
   ろ過the crystalline product was filtered off with suction
7. 7
   洗浄washed with water
8. 8
   その他dried

実験手順

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.

出典