反应详情

温度

0 °C

A 10 mL rb flask was charged with a solution of 0.075 g (0.13 mmol) of the product of Step A and 0.052 g (0.2 mmol) triphenylphosphine in 2 mL THF. The reaction mixture was stirred at 0° C. and 39 μL of diisopropylazodicarboxylate was added dropwise. The reaction mixture was stirred an additional 1 h at room temperature, then evaporated to dryness. The residue was purified on a silica gel flash chromatographic column eluted with 0–75% EtOAc-hexane. Evaporation of the purified fractions and drying in vacuo afforded the title compound. HPLC/MS: 550.0 (M+1), 551.9 (M+3); Rt=3.95 min.

1. stirringThe reaction mixture was stirred an additional 1 h at room temperature
2. customevaporated to dryness
3. customThe residue was purified on a silica gel flash chromatographic column
4. washeluted with 0–75% EtOAc-hexane
5. customEvaporation of the purified fractions
6. customdrying in vacuo