反应详情

温度

100 °C

To a pressure reaction flask containing diethyl malonate (4.1 mL, 27 mmol) in 50 mL of anhydrous dioxane was added NaH (1.1 g, 27.5 mmol, ˜60% in mineral oil) in several portions at RT, and stirred for 30 min. Compound 1E (2.5 g, 9 mmol) and CuI (5.1 g, 26.8 mmol) were added, sealed and heated at 100° C. for 3 days. The reaction was cooled to RT and filtered through a pad of celite. The celite pad was washed with EtOAc. The organics were washed twice with water, dried over Na2SO4, filtered and concentrated. Purification by flash chromatography (silica gel, 110 g ISCO, 10% EtOAc in hexane) gave the title compound (2.3 g).

1. customTo a pressure reaction flask
2. customsealed
3. temperatureThe reaction was cooled to RT
4. filtrationfiltered through a pad of celite
5. washThe celite pad was washed with EtOAc
6. washThe organics were washed twice with water
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. concentrationconcentrated
10. customPurification by flash chromatography (silica gel, 110 g ISCO, 10% EtOAc in hexane)