تفاعل #5099

ord-7a603da7931848aeaaadbcc3c883c330

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىthe solvent was removed by evaporation under a reduced pressure
  2. 2
    أخرىto the residue thus obtained
  3. 3
    درجة الحرارةcooled
  4. 4
    أخرىcrystallized
  5. 5
    ترشيحThe crystals were collected by filtration
  6. 6
    غسيلwashed with water
  7. 7
    أخرىrecrystallized from water

الإجراء التجريبي

200 Grams of 6-chloroacetylaminomethyl-2,3-dihydro-7-hydroxy-4-methyl-1H-indene-1-one, 77.9 g of hydroxylamine hydrochloride, 300 ml of pyridine and 1,800 ml of ethanol were refluxed for 3 hours. After the reaction was completed, the solvent was removed by evaporation under a reduced pressure, then to the residue thus obtained was added 2 liters of water and the mixture was stirred vigorously, cooled and crystallized. The crystals were collected by filtration, washed with water, and recrystallized from water to obtain 167 g of (2,3-dihydro-7-hydroxy-1-hydroxyimino-4-methyl-1H-indene-6yl)-methylaminocarbonylmethylpyridinium chloride. Colorless flake-like crystals. Melting point: 279° C. (Decomposed).

المصدر

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