Hydrochloric Acid → HCID 178447286, Verbindung

HRID 1609202Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1609202
[NH:1]1[C:5]([C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=2[C:12]2[CH:17]=[CH:16][C:15]([CH2:18][N:19]([CH2:26][C:27]([CH2:35][CH3:36])([CH2:33][CH3:34])[C:28]([O:30]CC)=[O:29])[C:20](=[O:25])[CH2:21][CH2:22][CH2:23][CH3:24])=[CH:14][CH:13]=2)=[N:4][N:3]=[N:2]1.[OH-].[Na+].Cl.C(Cl)Cl.CO>C(O)C>[C:28]([C:27]([CH2:35][CH3:36])([CH2:33][CH3:34])[CH2:26][N:19]([C:20](=[O:25])[CH2:21][CH2:22][CH2:23][CH3:24])[CH2:18][C:15]1[CH:14]=[CH:13][C:12]([C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[C:5]2[NH:1][N:2]=[N:3][N:4]=2)=[CH:17][CH:16]=1)([OH:30])=[O:29]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 21226129Dichloromethane methanolHCID 178447287HCID 178447287, Verbindung

Produkt 1

HCID 178447286HCID 178447286, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

1.146 g of ethyl N-[(2'-(1H-tetrazol-5-yl)biphenyl-4-yl)methyl]-N-valeryl-2-aminomethyl-2-ethylbutyrate are dissolved in 10 ml of ethanol, treated with 4.66 ml of 2N NaOH solution and heated to reflux for 20 hours. After cooling to room temperature and addition of 4.66 ml of 2N hydrochloric acid, the mixture is evaporated. The product is isolated by chromatography on silica gel 60 (40-63 μm) using CH2Cl2 -MeOH 80:20, Rf =0.38 (system N8). MS (FAB):m/e 486 (M+ +Na), 502 (M+ +K).

Aufarbeitung

  1. temperatureheated
  2. temperatureto reflux for 20 hours
  3. customthe mixture is evaporated
  4. customThe product is isolated by chromatography on silica gel 60 (40-63 μm)

Quellen und Nachweise

ORD-Eintrag
ord-7bbeb25c82b14a078faf62d75068e9ec
Quelldatensatz
uspto-grants-1995_03
Patentnummer
US05399578

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