Phosphorus oxychloride → HCID 18596278, Verbindung

HRID 615935Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 615935
P(Cl)(Cl)([Cl:3])=O.[NH2:6][C:7]1[N:8]=[C:9]([Cl:24])[C:10]2[CH2:19][C@H:18]3[C@@H:13]([CH2:14][CH2:15][CH2:16][N:17]3[CH2:20][CH2:21][CH3:22])[CH2:12][C:11]=2[N:23]=1>>[ClH:3].[NH2:6][C:7]1[N:8]=[C:9]([Cl:24])[C:10]2[CH2:19][C@H:18]3[C@@H:13]([CH2:14][CH2:15][CH2:16][N:17]3[CH2:20][CH2:21][CH3:22])[CH2:12][C:11]=2[N:23]=1

Komponenten

3

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 18596258HCID 18596258, Verbindung

Produkt 1

HCID 18596278HCID 18596278, Verbindung

Versuchsvorschrift

The 4-hydroxy product thus obtained was refluxed with 4 ml. of phosphorous oxychloride. The reaction mixture, containing trans-(±)-2-amino-4-chloro-6-n-propyl-5,5a,6,7,8,9,9a,10-octahydropyrimido[4,5-g]-quinoline formed in the above reaction, was poured onto ice and the resulting aqueous mixture made basic. The basic mixture was filtered and the insoluble material dissolved in 0.1N aqueous hydrochloric acid. The hydrochloride salt thus prepared was recrystallized from ethanol to yield trans-(±)-2-amino-4-chloro-6-n-propyl-5,5a,6,7,8,9,9a,10-octahydropyrimido[4,5-g]quinoline hydrochloride having the following physical characteristics. Mass spectrum, molecular ion at 280, smaller peak at 282.

Aufarbeitung

  1. temperaturewas refluxed with 4 ml
  2. customformed in the above reaction
  3. additionwas poured onto ice
  4. filtrationThe basic mixture was filtered
  5. dissolutionthe insoluble material dissolved in 0.1N aqueous hydrochloric acid
  6. customThe hydrochloride salt thus prepared
  7. customwas recrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-fa9dea4ed0f54267a2e47d9306cc0d3d
Quelldatensatz
uspto-grants-1985_02
Patentnummer
US04501890

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