반응 #170442

반응 방정식

4-fluoroacetophenone

ethyl trifluoroacetate

sodium methoxide

→

title compound

수율 97.0%

4,4,4-Trifluoro-1-(4-fluoro-phenyl)-butane-1,3-dione

수율 97.0%

용매

HCl

tertbutylmethylether

반응 조건

후처리

1. 1
   추출extracted with ethyl acetate
2. 2
   건조The combined organic extracts were then dried over sodium sulfate
3. 3
   기타evaporated

실험 절차

To a solution of ethyl trifluoroacetate (23.9 mL, 199 mmol) in tertbutylmethylether (230 mL) containing sodium methoxide (5.4 M, 39.6 mL, 214 mmol) was added 4-fluoroacetophenone (25 g, 181 mmol) and the resulting mixture stirred at room temperature for 3 h and then poured into ice-water. The mixture was then diluted with HCl (2 N, 200 mL) and then extracted with ethyl acetate. The combined organic extracts were then dried over sodium sulfate and evaporated to afford the title compound (40.9 g, 97%) which was obtained as an orange oil. MS: m/e=232.9 [M−H]−.

출처