반응 #2028867

반응 방정식

4′-Methylacetophenone

sodium methoxide

ethyl trifluoroacetate

→

brown oil

수율 94.0%

1-(4-methylphenyl)-4,4,4-trifluorobutane-1,3-dione

수율 94.0%

용매

methanol

methanol

반응 조건

후처리

1. 1
   온도After refluxing for 24 hours
2. 2
   농축concentrated
3. 3
   workup.ADDITION100 mL 10% HCl was added
4. 4
   추출the mixture extracted with 4×75 mL ethyl acetate
5. 5
   건조The extracts were dried over MgSO4
6. 6
   여과filtered
7. 7
   농축concentrated

실험 절차

4′-Methylacetophenone (5.26 g, 39.2 mmol) was dissolved in 25 mL of methanol under argon and 12 mL (52.5 mmol) sodium methoxide in methanol (25%) was added. The mixture was stirred for 5 minutes and 5.5 mL (46.2 mmol) ethyl trifluoroacetate was added. After refluxing for 24 hours, the mixture was cooled to room temperature and concentrated. 100 mL 10% HCl was added and the mixture extracted with 4×75 mL ethyl acetate. The extracts were dried over MgSO4, filtered and concentrated to afford 8.47 g (94%) of a brown oil which was carried on without further purification.

출처