反应详情

温度

0 °C

Diethyl cyanomethylphosphonate (1.15 eq.) is slowly added to a suspension of sodium hydride (1.15 eq.) in anhydrous tetrahydrofuran at 0° C. The reaction medium is stirred for 10 minutes at 0° C. and then cooled to −78° C. 4-Chromanone dissolved in tetrahydrofuran is added. The temperature is then returned slowly to 20-25° C. over 2 hours 30. After removal of the solvent, the compounds are extracted with ethyl acetate. The organic phase is washed with a large amount of a saturated solution of sodium chloride, concentrated and purified (Z/E mixture) on a silica column (AcOEt/PE 3/7).

1. temperaturecooled to −78° C
2. additionis added
3. waitThe temperature is then returned slowly to 20-25° C. over 2 hours
4. customAfter removal of the solvent
5. extractionthe compounds are extracted with ethyl acetate
6. washThe organic phase is washed with a large amount of a saturated solution of sodium chloride
7. concentrationconcentrated
8. custompurified (Z/E mixture) on a silica column (AcOEt/PE 3/7)