Ethanol → (2,3-dihydro-7-hydroxy-1-hydroxyimino-4-methyl-1H-indene-6-yl)methylaminocarbonylmethylpyridinium chloride

HRID 345137

Reaktionsgleichung

Reaktionsgleichung von HRID 345137
[Cl:1][CH2:2][C:3]([NH:5][CH2:6][C:7]1[C:15]([OH:16])=[C:14]2[C:10]([CH2:11][CH2:12][C:13]2=O)=[C:9]([CH3:18])[CH:8]=1)=[O:4].Cl.[NH2:20][OH:21].[N:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.C(O)C>O>[Cl-:1].[OH:16][C:15]1[C:7]([CH2:6][NH:5][C:3]([CH2:2][N+:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)=[O:4])=[CH:8][C:9]([CH3:18])=[C:10]2[C:14]=1[C:13](=[N:20][OH:21])[CH2:12][CH2:11]2

Komponenten

6

Edukt 4

HCID 702EthanolHCID 1049PyridineHCID 443297Hydroxyamine hydrochlorideHCID 136041414-Methyl-6-alpha-chloroacetylaminomethyl-7-hydroxy-1-indanone

Produkt 1

HCID 136364579(2,3-dihydro-7-hydroxy-1-hydroxyimino-4-methyl-1H-indene-6-yl)methylaminocarbonylmethylpyridinium chloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

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-6-yl)methylaminocarbonylmethylpyridinium chloride. Colorless flake-like crystals. Melting point: 279° C. (Decomposed).

Aufarbeitung

  1. customthe solvent was removed by evaporation under a reduced pressure
  2. customto the residue thus obtained
  3. temperaturecooled
  4. customcrystallized
  5. filtrationThe crystals were collected by filtration
  6. washwashed with water
  7. customrecrystallized from water

Quellen und Nachweise

ORD-Eintrag
ord-c0707d3ccdc843fe973022c3f7b11928
Quelldatensatz
uspto-grants-1991_10
Patentnummer
US05055474

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