反应详情

温度

80 °C

D2 (263 mg, 0.63 mmol) and N,N-diisopropylethylamine (111 μL, 0.63 mmol) were dissolved in acetic anhydride (10 mL) and heated to 80° C. The reaction stirred overnight. It was quenched with saturated aqueous sodium bicarbonate, then extracted with dichloromethane. The organic layer was washed with saturated aqueous sodium bicarbonate and brine, then dried over magnesium sulfate, filtered, concentrated in vacuo. Purified by chromatography (1:1 to 1:2 hexane:ethyl acetate), recovering 168 mg of D3.

1. customIt was quenched with saturated aqueous sodium bicarbonate
2. extractionextracted with dichloromethane
3. washThe organic layer was washed with saturated aqueous sodium bicarbonate and brine
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customPurified by chromatography (1:1 to 1:2 hexane:ethyl acetate)
8. customrecovering 168 mg of D3