Sodium Perchlorate → 6-Butylbenzo[b]quinolizinium perchlorate

HRID 742499Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 742499
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH:7]([C:9]1[C:14]([CH2:15]O)=[CH:13][CH:12]=[CH:11][C:10]=1CO)O.[Cl:19]([O-:23])(=[O:22])(=[O:21])=[O:20].[Na+]>O=P(Cl)(Cl)Cl>[Cl:19]([O-:23])(=[O:22])(=[O:21])=[O:20].[CH2:7]([C:15]1[N+:1]2[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=2[CH:7]=[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:14]=12)[CH2:2][CH2:3][CH3:4]

Komponenten

4

Edukt 2

HCID 522606Sodium PerchlorateHCID 117766291-(2-Pyridyl)-1-[2,6-di(hydroxymethyl)-phenyl]methanol

Produkt 1

HCID 190474766-Butylbenzo[b]quinolizinium perchlorate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 24813Phosphorus oxychlorideLösungsmittel

Versuchsvorschrift

A mixture of 0.6 g (2.5 mmol) of 1-(2-pyridyl)-1-[2,6-di(hydroxymethyl)-phenyl]methanol and 10 ml of POCl3 was refluxed with stirring for 4 hours. The mixture was cooled, poured onto ice, stirred and treated with a 20% sodium perchlorate solution. The resulting mixture was filtered, the resulting solid was washed with water, and dried to afford 0.58 g of 10-chloromethylrbenzo[b]quinolizinium perchlorate (Formula II: R1 =R2 =H; R7 =10--CH2Cl; X- =ClO4-).

Aufarbeitung

  1. temperaturewas refluxed
  2. temperatureThe mixture was cooled
  3. additionpoured onto ice
  4. stirringstirred
  5. filtrationThe resulting mixture was filtered
  6. washthe resulting solid was washed with water
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-429027ca47fc4447926e26a45f658d29
Quelldatensatz
uspto-grants-1996_09
Patentnummer
US05554620

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