반응 #45867

ord-76c1cd1e388e41eb867e36c7cd14dc26

반응 조건

온도
50°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도After cooling to room temperature
  2. 2
    기타the solvent was evaporated away under reduced pressure
  3. 3
    기타The residue was purified by middle-pressure liquid chromatography (eluent, n-hexane

실험 절차

At room temperature, Grubbs catalyst second generation (92 mg, 0.11 mol) was added to a solution of 7-(1-allylbut-3-enyl)-2-cyclopropyl-5-methyl-6-phenyl-1,3-benzoxazole-4-carbonitrile (I-299) (400 mg, 1.09 mmol) dissolved in dichloromethane; (108 ml). Under nitrogen atmosphere, the solution was stirred at 50° C. for 3.5 hours. After cooling to room temperature, the solvent was evaporated away under reduced pressure. The residue was purified by middle-pressure liquid chromatography (eluent, n-hexane:ethyl acetate=9:1, v/v) to obtain the entitled compound (282 mg, 76%) as a white solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07737166B2uspto-grants-2010_06