반응 #157822

ord-f0d6077fd2634ab992b6b6753c68aa16

반응 조건

온도
65°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과After filtration
  2. 2
    기타the solvent was evaporated under reduced pressure
  3. 3
    기타The resulting residue was purified by silica gel column chromatography (chloroform:methanol=1:0→95:5 9:1)

실험 절차

Water (0.2 mL) and 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (72 mg) were added to a solution of (5R)-5-[(E)-2-(4-tert-butylphenyl)-2-{5-methoxy-6-[(4-methoxybenzyl)oxy]-pyridin-2-yl}ethenyl]-1-(2,4-dimethoxybenzyl)pyrrolidin-2-one (202 mg) in chloroform (4 mL), and the mixture was stirred at 65° C. for 21 hours. Chloroform was added. After filtration, the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (chloroform:methanol=1:0→95:5 9:1) to give 6-{(E)-1-(4-tert-butylphenyl)-2-[(2R)-1-(2,4-dimethoxybenzyl)-5-oxopyrrolidin-2-yl]ethenyl}-3-methoxypyridin-2(1H)-one (65 mg).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08822503B2uspto-grants-2014_09