반응 #6789

반응 방정식

4-Methylthioacetophenone

ethyl trifluoroacetate

sodium methoxide

methanol

Hydrochloric acid

→

title compound

수율 71.0%

4,4,4-Trifluoro-1-[4-(methylthio)phenyl]butane-1,3-dione

수율 71.0%

용매

MTBE

반응 조건

후처리

1. 1
   기타the organic phase separated
2. 2
   세척washed with brine
3. 3
   건조dried (Na2SO4)
4. 4
   기타to give an orange solid
5. 5
   기타The orange solid was recrystallised from hot isopropanol

실험 절차

To a solution of ethyl trifluoroacetate (7.95 ml, 1.1 eq) in MTBE (125 ml) was added dropwise 25% sodium methoxide in methanol (16 ml, 1.2 eq). 4-Methylthioacetophenone (Aldrich, 10 g, 0.06 mol) was added portionwise and the mixture stirred at ambient temperature overnight. 2N Hydrochloric acid (40 ml) was added cautiously and the organic phase separated, washed with brine and dried (Na2SO4) to give an orange solid. The orange solid was recrystallised from hot isopropanol to give the title compound as a yellow crystalline solid (11.25 g, 71%).

출처