反应详情

温度

-15 °C

Compound (19) (300 mg, 0.583 mmol) was dissolved in dichloromethane (5.8 ml), and diethylaminosulfatrifluoride (DAST) was added to the solution with stirring under an argon stream at −15° C. The mixture was returned to room temperature 10 minutes after the addition of DAST and reacted for 1 hour. Disappearance of the material was confirmed by TLC, the DAST was quenched with methanol (3 ml), and the reaction mixture was concentrated in a vacuum. The residue was purified by silica gel chromatography (ethyl acetate:hexane=1:6), giving Compound (20) (in an amount of 211 mg, yield 70%).

1. customreacted for 1 hour
2. customthe DAST was quenched with methanol (3 ml)
3. concentrationthe reaction mixture was concentrated in a vacuum
4. customThe residue was purified by silica gel chromatography (ethyl acetate:hexane=1:6)