반응 #601851

반응 방정식

triethanolamine

Triphenylphosphine

DIAD

piperlongumine

→

desired product

수율 47.0%

(E)-N-methacryloylbut-2-enamide

수율 47.0%

용매

toluene

THF

반응 조건

후처리

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

실험 절차

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.

출처