反应详情

温度

-15 °C

Compound (20) (625 mg, 1.21 mmols) was dissolved in methanol (24.2 ml), and sodium methoxide (13.1 mg, 0.6 mmol) was added to the solution with stirring under an argon stream at −15° C. Disappearance of the material was confirmed by TLC 30 minutes later, and the reaction mixture was neutralized (pH 6-7) with a cation-exchange resin IR-120(+). After the resin was filtered off, the filtrate was concentrated in a vacuum. The residue was purified by silica gel chromatography (ethyl acetate:hexane=1:4), giving Compound (21) (in an amount of 395 mg, yield 74%).

1. customwas confirmed by TLC 30 minutes
2. filtrationAfter the resin was filtered off
3. concentrationthe filtrate was concentrated in a vacuum
4. customThe residue was purified by silica gel chromatography (ethyl acetate:hexane=1:4)