Sodium Hydroxide → HCID 23318332, Verbindung

HRID 1981974Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1981974
[CH3:1][N:2]1[CH2:23][CH2:22][N:5]2[C:6]3[CH:20]=[CH:19][C:18]([CH3:21])=[CH:17][C:7]=3[C:8]([C:12]3[O:13][CH:14]=[CH:15][CH:16]=3)=[N+:9]([O-])[CH2:10][CH:4]2[CH2:3]1.P(Cl)(Cl)[Cl:25].[OH-].[Na+]>C(Cl)(Cl)Cl>[CH3:1][N:2]1[CH2:23][CH2:22][N:5]2[C:6]3[CH:20]=[CH:19][C:18]([CH3:21])=[CH:17][C:7]=3[C:8]([C:12]3[O:13][C:14]([Cl:25])=[CH:15][CH:16]=3)=[N:9][CH2:10][CH:4]2[CH2:3]1

Komponenten

5

Edukt 3

HCID 14798Sodium HydroxideHCID 24387Phosphorus trichlorideHCID 30712577-(Furan-2-yl)-3,9-dimethyl-6-oxo-1,2,3,4,4a,5-hexahydro-6lambda~5~-pyrazino[1,2-a][1,4]benzodiazepine

Produkt 1

HCID 23318332HCID 23318332, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

9.3 g of 1,2,3,4,4a,5-hexahydro-3,9-dimethyl-7-(2-furyl)-pyrazino[1,2-a][1,4]benzodiazepine 6-oxide (prepared analogously to Example 5) are heated under reflux in 150 ml of chloroform with 17 ml of phosphorus trichloride for 1 hour. The reaction mixture is then treated with aqueous sodium hydroxide solution and worked up. The resulting crude product is separated into its components by chromatography on aluminium oxide of activity level II, using methylene chloride/chloroform. 1.7 g of the less polar 1,2,3,4,4a,5-hexahydro-3,9-dimethyl-7-(5-chloro-2-furyl)-pyrazino[1,2-a][1,4]benzodiazepine are thereby initially obtained in the first fraction, and the product is isolated as an oil (IR: 1,615 cm-1C=N) (b). 5 g of the more highly polar 1,2,3,4,4a,5-hexahydro-3,9-dimethyl-7-(2-furyl)-pyrazino[1,2-a][1,4]benzodiazepine (a) are then obtained.

Aufarbeitung

  1. temperatureare heated
  2. customThe resulting crude product is separated into its components by chromatography on aluminium oxide of activity level II

Quellen und Nachweise

ORD-Eintrag
ord-847b2a73de7243b3981f322096bdc0be
Quelldatensatz
uspto-grants-1986_06
Patentnummer
US04594436

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