Sodium Thiosulfate → UK-333747

HRID 2270925Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2270925
[Cl:1][C:2]1[C:3]([N:15]2[C:19]([C:20]3[CH:21]=[N:22][CH:23]=[CH:24][CH:25]=3)=[N:18][N:17]=[C:16]2[CH2:26][O:27][CH3:28])=[C:4]2[C:9](=[CH:10][C:11]=1[Cl:12])[NH:8][C:7](=[O:13])[C:6](=[O:14])[NH:5]2.[OH:29]OS([O-])=O.[K+].S([O-])([O-])(=O)=S.[Na+].[Na+]>O>[Cl:1][C:2]1[C:3]([N:15]2[C:19]([C:20]3[CH:21]=[N+:22]([O-:29])[CH:23]=[CH:24][CH:25]=3)=[N:18][N:17]=[C:16]2[CH2:26][O:27][CH3:28])=[C:4]2[C:9](=[CH:10][C:11]=1[Cl:12])[NH:8][C:7](=[O:13])[C:6](=[O:14])[NH:5]2

Komponenten

5

Edukt 3

HCID 24477Sodium ThiosulfateHCID 9802164HCID 9802164, VerbindungHCID 23707502Potassium hydroxy sulfite

Produkt 1

HCID 9867605UK-333747Ausbeute 85,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

(−)-6,7-Dichloro-5-[3-methoxymethyl-5-(3-pyridyl)-4H-1,2,4-triazol-4-yl]-2,3(1H,4H)-quinoxalinedione (see Preparation 1) (412.2 g, 0.98 mol) and OXONE (trade mark) (1.44 kg, 2.3 mol) were slurried in water (4.13 L) and the mixture stirred at ambient temperature for 60 hours. Saturated aqueous sodium thiosulphate solution (2.2 L) was added and the slurry stirred for 1 hour before being filtered under reduced pressure. The filter cake was slurried at ambient temperature for 4 hours in 1:1, by volume, isopropyl alcohol: dichloromethane (111 L) and the solid collected by filtration. The filtrate was vaporated under reduced pressure to give the title compound as a colourless solid (366 g).

Aufarbeitung

  1. stirringthe slurry stirred for 1 hour
  2. filtrationbefore being filtered under reduced pressure
  3. waitThe filter cake was slurried at ambient temperature for 4 hours in 1:1, by volume, isopropyl alcohol
  4. filtrationdichloromethane (111 L) and the solid collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-d0ef3a47acb04335804b7fb10422c28d
Quelldatensatz
uspto-grants-2001_12
Patentnummer
US06333326B1

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