Hydrochloric Acid → HCID 178447284, Verbindung

HRID 1739080Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1739080
[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]([C:29](=O)[CH2:30][CH2:31][CH2:32][CH3:33])[C:20]3(C([O-])=O)[CH2:24][CH2:23][CH2:22][CH:21]3[CH3:25])=[CH:14][CH:13]=2)=[N:4][N:3]=[N:2]1.[OH-:35].[Na+].Cl.C(Cl)Cl.[CH3:41][OH:42].C([OH:45])C>>[NH:1]1[C:5]([C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=2[C:12]2[CH:13]=[CH:14][C:15]([CH2:18][N:19]([CH2:20][C:24]3([C:41]([OH:45])=[O:42])[CH2:25][CH2:21][CH2:22][CH2:23]3)[C:29](=[O:35])[CH2:30][CH2:31][CH2:32][CH3:33])=[CH:16][CH:17]=2)=[N:4][N:3]=[N:2]1

Komponenten

6

Edukt 5

HCID 313Hydrochloric AcidHCID 702EthanolHCID 14798Sodium HydroxideHCID 21226129Dichloromethane methanolHCID 178447282HCID 178447282, Verbindung

Produkt 1

HCID 178447284HCID 178447284, Verbindung

Versuchsvorschrift

0.979 g of N-[(2'-(1H-tetrazol-5-yl)biphenyl-4-yl)methyl]-N-valeryl-1-amino-methylcyclopentane-1-carboxylate are dissolved in 10 ml of ethanol and treated with 4 ml of 2N NaOH solution, and the mixture is heated to reflux for 23 h. After cooling to room temperature and adding 4.5 ml of 2N hydrochloric acid, the mixture is evaporated and the product is isolated by chromatography on silica gel 60 (40-63 μm) using CH2Cl2 --MeOH 95:5, Rf =0.35 (system N8). MS (FAB): m/e 462 (M+ +H).

Aufarbeitung

  1. temperaturethe mixture is heated
  2. temperatureto reflux for 23 h
  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-901f824275714f8087597d3fa7f5e077
Quelldatensatz
uspto-grants-1999_10
Patentnummer
US05965592

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