반응 #1843

반응 방정식

potassium tert-butylate

trifluoroethanol

4,5-dichloro-2-nitrotoluene

→

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

반응 조건

후처리

1. 1
   온도cooling
2. 2
   온도the mixture was heated to 80°-90° C
3. 3
   온도After cooling
4. 4
   workup.STIRRINGthe mixture was stirred at 105° C. for 1 hour
5. 5
   농축It was concentrated in vacuo
6. 6
   workup.ADDITIONthe residue was treated with 300 ml of water
7. 7
   기타to give
8. 8
   여과after filtration with suction, 12 g of crude product, which
9. 9
   기타were purified over silica gel with n-heptane/ethyl acetate, 10 g of product, melting point 76°-79° C.

실험 절차

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.

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