반응 #81665

ord-3e05036fcc3340968a6d94747270326f

반응 조건

온도
80°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도cooled to room temperature
  2. 2
    농축concentrated in vacuo to an oil
  3. 3
    기타Purification by flash chromatography (silica, 10% EtOAc-hexane)

실험 절차

To 200 mg (0.51 mmol) of ethyl 4-[(5,6,7,8-tetrahydro-8,8-dimethyl-5-oxonapth-2-yl)ethynyl]benzoate (Compound 1) was added 0.13 ml (1.5 mmol) of acetic anhydride and 10 mg (0.05 mmol) of p-toluenesulfonic acid. The mixture was heated at 80° C. for 12 hours, cooled to room temperature and concentrated in vacuo to an oil. Purification by flash chromatography (silica, 10% EtOAc-hexane) yielded the title compound as a light yellow powder.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05618931uspto-grants-1997_04