反应详情

A solution of Intermediate 2 (5.0 g) in THF (20 ml) was added with diethyl azodicarboxylate (4.1 g, Ald), triphenylphosphine (8.0 g, WAKO), and methanol (990 μl, KANTO), and stirred for 4 hours. The reaction mixture was added with water (100 ml) and dichloromethane (20 ml×2) and extracted, the organic layer was successively washed with saturated aqueous sodium hydrogencarbonate, saturated aqueous ammonium chloride, and saturated brine, and dried, and the solvent was evaporated under reduced pressure. The residue was purified by column chromatography (Yamazen, n-hexane:ethyl acetate=3:1) to obtain the title compound (3.0 g).

1. extractionextracted
2. washthe organic layer was successively washed with saturated aqueous sodium hydrogencarbonate, saturated aqueous ammonium chloride, and saturated brine
3. customdried
4. customthe solvent was evaporated under reduced pressure
5. customThe residue was purified by column chromatography (Yamazen, n-hexane:ethyl acetate=3:1)