反应详情

A solution of diisopropyl azodicarboxylate (1.9 M in toluene, 2.20 mL) was added dropwise to a solution of diastereomer of 6-(6-(methoxymethoxy)-2-methyl-2,3-dihydrobenzofuran-2-yl)pyridin-3-ol (shorter retention time, 800 mg), (S)-tert-butyl (1-hydroxypropan-2-yl)carbamate (976 mg), and triphenylphosphine (1100 mg) in toluene (20 mL) at ambient temperature. The mixture was stirred at room temperature for 2 hr. The mixture was concentrated under reduced pressure. The residue was partitioned between ethyl acetate and water. The separated organic layer was washed with brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by column chromatography (hexane/ethyl acetate) to give the title compound (1100 mg).

1. concentrationThe mixture was concentrated under reduced pressure
2. customThe residue was partitioned between ethyl acetate and water
3. washThe separated organic layer was washed with brine
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by column chromatography (hexane/ethyl acetate)