反応 #1843

反応方程式

potassium tert-butylate

trifluoroethanol

4,5-dichloro-2-nitrotoluene

→

4-Chloro-2-nitro-5-(2,2,2-trifluoroethyloxy)toluene

反応条件

後処理

1. 1
   温度cooling
2. 2
   温度the mixture was heated to 80°-90° C
3. 3
   温度After cooling
4. 4
   workup.STIRRINGthe mixture was stirred at 105° C. for 1 hour
5. 5
   濃縮It was concentrated in vacuo
6. 6
   workup.ADDITIONthe residue was treated with 300 ml of water
7. 7
   その他to give
8. 8
   ろ過after filtration with suction, 12 g of crude product, which
9. 9
   その他were purified over silica gel with n-heptane/ethyl acetate, 10 g of product, melting point 76°-79° C.

実験手順

40.4 g (360 mmol) of potassium tert-butylate were added in portions to 60 ml of trifluoroethanol, while stirring and cooling, and the mixture was heated to 80°-90° C. After cooling, 14.4 g (70 mmol) of 4,5-dichloro-2-nitrotoluene were added and the mixture was stirred at 105° C. for 1 hour. It was concentrated in vacuo and the residue was treated with 300 ml of water to give, after filtration with suction, 12 g of crude product, which were purified over silica gel with n-heptane/ethyl acetate, 10 g of product, melting point 76°-79° C.

出典