反应详情

To a cooled (0° C.) solution of (4-((1,3-dioxolan-2-yl)methyl)phenyl)methanol (0.45 g, 2.317 mmol), 3-hydroxybenzophenone (0.551 g, 2.78 mmol) and triphenylphosphine (0.729 g, 2.78 mmol) in anhydrous THF, di-iso-propylazodicarboxylate (1.027 mL, 2.78 mmol) was added dropwise. The reaction mixture was allowed to warm to RT and stirred at this temperature for 16 hours. The reaction mixture was diluted with ethyl acetate and washed with 10% aqueous potassium carbonate, brine and dried (magnesium sulfate). The suspension was filtered and concentrated under reduced pressure. The crude material was purified by silica gel chromatography eluting with 100% iso-hexane to 25% ethyl acetate in iso-hexane to afford the title compound (1.022 g, >100%).

1. additionwas added dropwise
2. washwashed with 10% aqueous potassium carbonate, brine
3. dry with materialdried (magnesium sulfate)
4. filtrationThe suspension was filtered
5. concentrationconcentrated under reduced pressure
6. customThe crude material was purified by silica gel chromatography
7. washeluting with 100% iso-hexane to 25% ethyl acetate in iso-hexane