反応 #2028867

反応方程式

4′-Methylacetophenone

sodium methoxide

ethyl trifluoroacetate

→

brown oil

収率 94.0%

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

収率 94.0%

溶媒

methanol

methanol

反応条件

後処理

1. 1
   温度After refluxing for 24 hours
2. 2
   濃縮concentrated
3. 3
   workup.ADDITION100 mL 10% HCl was added
4. 4
   抽出the mixture extracted with 4×75 mL ethyl acetate
5. 5
   乾燥The extracts were dried over MgSO4
6. 6
   ろ過filtered
7. 7
   濃縮concentrated

実験手順

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.

出典