Ethanol → 6-Nitro-4-chromanone Oxime

HRID 1764117

Reaktionsgleichung

Reaktionsgleichung von HRID 1764117
Cl.[NH2:2][OH:3].[OH-].[Na+].[N+:6]([C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[O:15][CH2:14][CH2:13][C:12]2=O)([O-:8])=[O:7].C(O)C>O>[N+:6]([C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[O:15][CH2:14][CH2:13][C:12]2=[N:2][OH:3])([O-:8])=[O:7]

Komponenten

6

Edukt 4

HCID 702EthanolHCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 52288316-nitro-3,4-dihydro-2H-1-benzopyran-4-one

Produkt 1

HCID 859699586-Nitro-4-chromanone Oxime

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A solution of 79 g (1.14 mole) of hydroxylamine hydrochloride in 770 ml of H2O, contained in a 2 l. Erlenmeyer flask, was treated with 619 ml of 10% NaOH, 150 g (0.78 mole) of 6-nitro-4-chromanone and enough ethanol (750 ml) to produce a solution at the boiling point. The reaction mixture was boiled for 25 min., cooled to 50° over 2 hrs., and filtered. The filtrate was refrigerated overnight and filtered. The tan crystalline solid was washed with 200 ml of ethanol and dried, m.p. 173°-178°. Yield: 60 g (37%).

Aufarbeitung

  1. customto produce a solution at the boiling point
  2. temperaturecooled to 50° over 2 hrs
  3. filtration, and filtered
  4. waitThe filtrate was refrigerated overnight
  5. filtrationfiltered
  6. washThe tan crystalline solid was washed with 200 ml of ethanol
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-d64b3536d9a641eaa5934ddf2e7e49a1
Quelldatensatz
uspto-grants-1978_09
Patentnummer
US04115405

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