تفاعل #943179

ord-5b5db85593b541c8898bb30278d9f8c9

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe reaction mixture was heated
  2. 2
    درجة الحرارةat reflux for 24 h
  3. 3
    درجة الحرارةthe reaction mixture was heated
  4. 4
    درجة الحرارةat reflux for 24 h
  5. 5
    غسيلThe ethyl acetate solution was washed sequentially with 25 ml water and 25 ml brine
  6. 6
    تجفيفdried (anhydrous sodium sulfate)
  7. 7
    تركيزconcentrated under reduced pressure
  8. 8
    أخرىThe crude product was purified by column chromatography (silica gel)
  9. 9
    غسيلeluting with 14:1 hexane/ethyl acetate

الإجراء التجريبي

To a solution of 4-hydroxy-4′nitrobiphenyl in 5 ml acetone was added potassium carbonate (240 mg, 1.74 mmol) and 1-iodopropane (0.17 ml, 1.74 mmol). The reaction mixture was heated at reflux for 24 h. Additional potassium carbonate (240 mg, 1.74 mmol) and 1-iodopropane (0.17 ml, 1.74 mmol) was added and the reaction mixture was heated at reflux for 24 h. The reaction mixture was cooled to room temperature and diluted with 30 ml ethyl acetate. The ethyl acetate solution was washed sequentially with 25 ml water and 25 ml brine, dried (anhydrous sodium sulfate) and concentrated under reduced pressure. The crude product was purified by column chromatography (silica gel), eluting with 14:1 hexane/ethyl acetate to yield the title compound (0.267 g, 89% yield) MS: 258.3 (M−1)

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07262318B2uspto-grants-2007_08