تفاعل #5097

ord-8a19649ebcff469e91efc72f600ed2a4

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas refluxed for 4 hours
  2. 2
    تركيزthe reaction mixture was concentrated to dryness under a reduced pressure
  3. 3
    أخرىthe residue thus obtained
  4. 4
    غسيلwashed three times with 1 liter of water each time
  5. 5
    أخرىthe residue was dried again under a reduced pressure
  6. 6
    أخرىRecrystallized from ethyl acetate/n-hexane mixture

الإجراء التجريبي

An ethanol solution containing 120 g of 2,3-dihydro-7-hydroxy-4-methyl-6-(1-phenyl-2-propenyl)-1H-inden-1-one, 45 of hydroxylamine hydrochloride and 200 ml of pyridine in 1,200 ml of ethanol was refluxed for 4 hours. After the reaction was completed, the reaction mixture was concentrated to dryness under a reduced pressure, then the residue thus obtained was dissolved in 2 liters of ethyl acetate and washed three times with 1 liter of water each time, and the residue was dried again under a reduced pressure. Recrystallized from ethyl acetate/n-hexane mixture to obtain 90 g of 2,3-dihydro-7-hydroxy-4-methyl-6-(1-phenyl-2-propenyl)-1H-inden-1-one oxime. Light yellow flake-like crystals. Melting point: 146° C. (Decomposed).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05242919uspto-grants-1993_09