Hydrochloric Acid → HCID 67780906, Verbindung

HRID 2260149Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2260149
[OH-].[Na+].[CH2:3]1[C@H:8]2[C:9]3[CH:21]=[CH:20][CH:19]=[CH:18][C:10]=3[CH2:11][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[N:7]2[CH2:6][CH2:5][N:4]1[CH2:22][CH2:23][CH2:24][C:25]([O:27]CC)=[O:26].[ClH:30]>C(O)C>[ClH:30].[CH2:3]1[C@H:8]2[C:9]3[CH:21]=[CH:20][CH:19]=[CH:18][C:10]=3[CH2:11][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[N:7]2[CH2:6][CH2:5][N:4]1[CH2:22][CH2:23][CH2:24][C:25]([OH:27])=[O:26]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 15287790HCID 15287790, Verbindung

Produkt 1

HCID 67780906HCID 67780906, VerbindungAusbeute 76 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

20 ml of a 10% w/v aqueous solution of sodium hydroxide were added to a solution of 14.34 g of ethyl (R)-4-(1,2,3,4,10,14b-hexahydrodibenzo[c,f]pyrazino[1.2-a]azepin-2-yl)butyrate (prepared as described in Example 5") in 100 ml of ethanol, and the resulting mixture was stirred at room temperature for 1 hour. At the end of this time, the pH of the reaction mixture was adjusted to a value of 2 by the addition of 10% w/v aqueous hydrochloric acid, and the solvent was removed by distillation under reduced pressure. The crystals which precipitated were collected by filtration and dried, to give the title compound, melting at 265°-268° C. (with decomposition), in a 76% yield.

Aufarbeitung

  1. additionAt the end of this time, the pH of the reaction mixture was adjusted to a value of 2 by the addition of 10%
  2. customthe solvent was removed by distillation under reduced pressure
  3. customThe crystals which precipitated
  4. filtrationwere collected by filtration
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-845d02361f32441cb86e9af3510fe563
Quelldatensatz
uspto-grants-1995_12
Patentnummer
US05476848

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