تفاعل #81665

ord-3e05036fcc3340968a6d94747270326f

ظروف التفاعل

درجة الحرارة
80°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةcooled to room temperature
  2. 2
    تركيزconcentrated in vacuo to an oil
  3. 3
    أخرىPurification by flash chromatography (silica, 10% EtOAc-hexane)

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05618931uspto-grants-1997_04