Ethanol → HCID 136342833, Verbindung

HRID 2232205

Reaktionsgleichung

Reaktionsgleichung von HRID 2232205
[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.Cl.[NH2:20][OH:21].[N:22]1[CH:27]=[CH:26]C=C[CH:23]=1.[CH2:28](O)[CH3:29].[OH2:31]>>[Cl-:1].[OH:16][C:15]1[C:7]([C:6]2[CH:29]=[CH:28][CH:2]=[CH:3][N+:5]=2[CH2:26][C:27]([NH:22][CH3:23])=[O:31])=[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 5

HCID 702EthanolHCID 962WaterHCID 1049PyridineHCID 443297Hydroxyamine hydrochlorideHCID 136041414-Methyl-6-alpha-chloroacetylaminomethyl-7-hydroxy-1-indanone

Produkt 1

HCID 136342833HCID 136342833, Verbindung

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-9da84f27b5424d6c987c0a1b819968f2
Quelldatensatz
uspto-grants-1988_11
Patentnummer
US04788130

Verknüpfte Notizen

Wird geladen…