反应详情

温度

25 °C

To a suspension of sodium hydride (NaH; 0.13 g, 5.4 mmol) in 5 mL of anhydrous tetrahydrofuran (THF) was added ethyl trifluoracetate (CF3COOEt; 0.64 g, 4.5 mmol) under argon. After stirring at 25° C. for 10 minutes, 2-acetylphenanthrene (1 g, 4.5 mmol) in 5 mL of THF was added dropwise to the solution. The mixture became clear and orange-hued within 30 minutes, and after stirring for an additional 2 hours, was concentrated under vacuum. The residue was suspended in water, and extracted with ethyl acetate (15 mL) twice. The organic phase was separated, dried over sodium sulfate, and concentrated to dryness under vacuum to give the product (yellow solid; 1.29 g, 90% yield). The product was used directly without further purification.

1. waitThe mixture became clear and orange-hued within 30 minutes
2. stirringafter stirring for an additional 2 hours
3. concentrationwas concentrated under vacuum
4. extractionextracted with ethyl acetate (15 mL) twice
5. customThe organic phase was separated
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated to dryness under vacuum
8. customto give the product (yellow solid; 1.29 g, 90% yield)
9. customThe product was used directly without further purification