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Hydrochloric Acid → HCID 11058732, Verbindung

HRID 1870259
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1870259
C[C@@H]([O:8][C:9]([CH2:11][C@@H:12]1[C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=2[N:16]([C:23](=[O:36])[C:24]2[CH:29]=[CH:28][C:27]([N:30]3[CH2:34][CH2:33][CH2:32][CH2:31]3)=[CH:26][C:25]=2[Cl:35])[CH2:15][CH2:14][CH2:13]1)=[O:10])CCCCC.[OH-].[Na+].Cl>CO>[C:9]([CH2:11][C@@H:12]1[C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=2[N:16]([C:23](=[O:36])[C:24]2[CH:29]=[CH:28][C:27]([N:30]3[CH2:31][CH2:32][CH2:33][CH2:34]3)=[CH:26][C:25]=2[Cl:35])[CH2:15][CH2:14][CH2:13]1)([OH:10])=[O:8]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 14798Sodium Hydroxide2×HCID 10973260HCID 10973260, Verbindung

Produkt 1

HCID 11058732HCID 11058732, VerbindungAusbeute 79,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
45 °C

Versuchsvorschrift

To a suspension of (5R)-5-((R)-2-heptyloxycarbonylmethyl)-1-[4-(1-pyrrolidinyl)-2-chlorobenzoyl]-2,3,4,5-tetrahydro-1H-benzazepine (33 g) in methanol (500 ml) is added a 5N aqueous sodium hydroxide solution (25.8 ml), and the mixture is heated with stirring at 40-50° C. for two hours. To the mixture is further added a 5N aqueous sodium hydroxide solution (15 ml), and the mixture is heated with stirring at 50° C. for three hours. The reaction solution is acidified with hydrochloric acid, and concentrated under reduced pressure to remove the methanol, and extracted with ethyl acetate. The ethyl acetate layer is washed with water, dried over magnesium sulfate, and concentrated under reduced pressure to remove the ethyl acetate. The resultant is crystallized from ethyl acetate--diethyl ether, washed with diethyl ether--n-hexane to give (5R)-5-carboxymethyl-1-[4-(1-pyrrolidinyl)-2-chlorobenzoyl]-2,3,4,5-tetrahydro-1H-benzazepine (21.1 g).

Aufarbeitung

  1. temperaturethe mixture is heated
  2. temperaturethe mixture is heated
  3. stirringwith stirring at 50° C. for three hours
  4. concentrationconcentrated under reduced pressure
  5. customto remove the methanol
  6. extractionextracted with ethyl acetate
  7. washThe ethyl acetate layer is washed with water
  8. dry with materialdried over magnesium sulfate
  9. concentrationconcentrated under reduced pressure
  10. customto remove the ethyl acetate
  11. customThe resultant is crystallized from ethyl acetate
  12. washdiethyl ether, washed with diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-290e5f27099b44e2b7aa60126adeee46
Quelldatensatz
uspto-grants-2000_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06096736

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