反应详情

To 6-2 (2.12 g, 10.0 mmol) in tetrahydrofuran (25 ml) under a nitrogen atmosphere was added ethyl 4-hydroxybenzoate (6-3) (1.66 g, 10.0 mmol) followed by triphenyl phosphine (3.15 g, 12.0 mmol). The mixture was cooled in an ice bath and diethyl azodicarboxylate (2.09 g, 12 mmol) was added. This mixture was stirred overnight at ambient temperature and the solvent was removed in vacuo. The residue was taken up in the water and the ether layer was separated, washed with sodium bicarbonate and water, dried, filtered and concentrated in vacuo to yield an oil. Chromatographic purification on silica gel gave 6-4 as a colorless oil.

1. temperatureThe mixture was cooled in an ice bath
2. customthe solvent was removed in vacuo
3. customthe ether layer was separated
4. washwashed with sodium bicarbonate and water
5. customdried
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customto yield an oil
9. customChromatographic purification on silica gel