تفاعل #47829

ord-ef70888cc8144573b9748559881916f2

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةrefluxed for 1 hr
  2. 2
    غسيلThe resulting mixture washed with saturated sodium bicarbonate
  3. 3
    استخلاصextracted with ethyl acetate
  4. 4
    أخرىThe organic layer was separated
  5. 5
    تجفيفdried over anhydrous MgSO4
  6. 6
    تركيزconcentrated under a reduced pressure
  7. 7
    أخرىThe resulting residue was purified by flash chromatography

الإجراء التجريبي

1-Oxo-3-phenyl-6-(3-phenyl-propoxy)-1H-indene-2-carboxylic acid ethyl ester (1.5 g, 3.64 mmol) obtained in Example 7 was dissolved in ethanol (100 mL), hydroxylamine hydrochloride (759 mg, 10.92 mmol) and pyridine (1.15 g, 15.56 mmol) were added thereto, refluxed for 1 hr, and cooled to RT. The resulting mixture washed with saturated sodium bicarbonate and extracted with ethyl acetate. The organic layer was separated, dried over anhydrous MgSO4 and concentrated under a reduced pressure. The resulting residue was purified by flash chromatography to obtain 0.91 g of the titled compound (yield: 58%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07745439B2uspto-grants-2010_06