反应详情

Experimental Procedure: Triphenylphosphine (79.0 mg, 0.30 mmol) and DIAD (61.0 mg, 0.30 mmol) were dissolved to a 1:1 mixture of THF and toluene (2 mL); then mono-demethylated piperlongumine (46.0 mg, 0.15 mmol) was added. After 10 min, triethanolamine (6.80 mg, 0.05 mmol) was added to the mixture. The reaction was stirred at room temperature for 3 h. At the end, the solvent was evaporated under vacuum. The crude product was purified by preparative TLC(CH2Cl2/MeOH=9/1) to afford the desired product in 47% yield.

1. customAt the end, the solvent was evaporated under vacuum
2. customThe crude product was purified by preparative TLC(CH2Cl2/MeOH=9/1)