反应详情

After drying 4-(2-hydroxyethoxy)-6-methylpyridin-3-ol (714 mg, 4.22 mmol) and triphenylphosphine (1.66 g, 6.33 mmol) with a vacuum pump, the resultant was dissolved in tetrahydrofuran (42 mL), added di-tert-butyl azodicarboxylate (DBAD) (1.46 g, 6.33 mmol) under ice-cold conditions, and the mixture was stirred at room temperature overnight. Under ice-cold conditions, the reaction solution was added water, and extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous sodium sulfate, and concentrated in vacuo. The obtained residue was purified by silica-gel column chromatography (hexane/acetone, chloroform/methanol). The title compound (1.74 g (yield >100%)) was obtained as a white solid as a crude product.

1. extractionextracted with ethyl acetate
2. washThe organic layer was washed with brine
3. dry with materialdried over anhydrous sodium sulfate
4. concentrationconcentrated in vacuo
5. customThe obtained residue was purified by silica-gel column chromatography (hexane/acetone, chloroform/methanol)