反应详情

温度

0 °C

Triphenylphosphene (3.6 g, 13.76 mmol) and diethyl azodicarboxylate (2.2 mL, 13.76 mmol) were dissolved in THF (10 mL) and cooled to 0° C. To this was added a solution of the product from Step A (1.9 g, 8.6 mmol) in THF (10 mL) and the mixture was stirred at 0° C. for 3 hr. The solvent was evaporated and the residue dissolved in ethyl acetate (100 mL); this solution was washed with water (2×50 mL) and brine (2×50 mL), dried (MgSO4), and evaporated to a syrup which was purified by column chromatography (silica, 1:2 hexane/ethyl acetate) to give the desired product (995 mg, 57%).

1. customThe solvent was evaporated
2. dissolutionthe residue dissolved in ethyl acetate (100 mL)
3. washthis solution was washed with water (2×50 mL) and brine (2×50 mL)
4. dry with materialdried (MgSO4)
5. customevaporated to a syrup which
6. customwas purified by column chromatography (silica, 1:2 hexane/ethyl acetate)