Water → HCID 86615652, Verbindung

HRID 507020Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 507020
[C:1](N1C=CN=C1)#[N:2].[F:8][C:9]([F:41])([F:40])[C:10]1[CH:11]=[C:12]([CH:33]=[C:34]([C:36]([F:39])([F:38])[F:37])[CH:35]=1)[CH2:13][NH:14][CH:15]1[CH2:21][CH2:20][CH2:19][N:18]([C:22]([O:24][CH:25]([CH3:27])[CH3:26])=[O:23])[C:17]2[CH:28]=[CH:29][C:30]([Br:32])=[CH:31][C:16]1=2.O>CN(C)C(=O)C>[F:41][C:9]([F:8])([F:40])[C:10]1[CH:11]=[C:12]([CH:33]=[C:34]([C:36]([F:37])([F:38])[F:39])[CH:35]=1)[CH2:13][N:14]([C:1]#[N:2])[CH:15]1[CH2:21][CH2:20][CH2:19][N:18]([C:22]([O:24][CH:25]([CH3:27])[CH3:26])=[O:23])[C:17]2[CH:28]=[CH:29][C:30]([Br:32])=[CH:31][C:16]1=2

Komponenten

5

Edukt 3

HCID 962WaterHCID 2735857N-CyanoimidazoleHCID 59432351HCID 59432351, Verbindung

Produkt 1

HCID 86615652HCID 86615652, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 31374DimethylacetamideLösungsmittel2×

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

Add a solution of 1-cyanoimidazole in N,N-dimethylacetamide to a solution of isopropyl 5-(3,5-bistrifluoromethylbenzylamino)-7-bromo-2,3,4,5-tetrahydrobenzo[b]azepine-1-carboxylate in N,N-dimethylacetamide at room temperature under nitrogen and heat the mixture to 100° C. Pour the cooled mixture into water and extract with methylene chloride. Dry the organic layer over anhydrous sodium sulfate, filter, and remove the solvent under reduced pressure. Chromatograph the residue over silica gel to afford the title compound.

Aufarbeitung

  1. extractionextract with methylene chloride
  2. dry with materialDry the organic layer over anhydrous sodium sulfate
  3. filtrationfilter
  4. customremove the solvent under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-9fcf7ffc2bb34b519322fade31ce38ae
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07786108B2

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