1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 10385550, Verbindung

HRID 1242885Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1242885
CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1.[CH3:22][N:23]([CH3:27])[CH2:24][CH2:25][NH2:26].[C:28]1([C:46]2[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=2)[CH:33]=[CH:32][C:31]([C:34]([NH:36][C:37]2[CH:45]=[CH:44][C:40]([C:41]([O-])=[O:42])=[CH:39][CH:38]=2)=[O:35])=[CH:30][CH:29]=1>C1COCC1.C(#N)C.C(OCC)(=O)C.O.C(N(CC)CC)C>[CH3:22][N:23]([CH3:27])[CH2:24][CH2:25][NH:26][C:41]([C:40]1[CH:39]=[CH:38][C:37]([NH:36][C:34]([C:31]2[CH:32]=[CH:33][C:28]([C:46]3[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=3)=[CH:29][CH:30]=2)=[O:35])=[CH:45][CH:44]=1)=[O:42]

Komponenten

10

Edukt 4

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 66053N,N-DimethylethylenediamineHCID 757711-HydroxybenzotriazoleHCID 7040114HCID 7040114, Verbindung

Produkt 1

HCID 10385550HCID 10385550, VerbindungAusbeute 25,3 %

Reagenzien, Katalysatoren, Lösungsmittel 5

HCID 962WaterLösungsmittelHCID 6342AcetonitrileLösungsmittelHCID 8028TetrahydrofuranLösungsmittelHCID 8471TriethylamineLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

WSC (0.248 g), HOBt (0.156 g), N,N-dimethyl ethylenediamine (0.097 g) and triethylamine (0.21 ml) were added to a mixed solution of 4-(4-biphenylylcarbonylamino)benzoate (0.323 g) in THF (15 ml) and acetonitrile (15 ml). After stirring at room temperature for 18 hours, water was added to the reaction mixture, and extraction was conducted using ethyl acetate. The organic layer was washed with 10% aqueous potassium carbonate and saturated aqueous sodium chloride solution, dried, and then concentrated. The residue was recrystallized using methanol/diethyl ether to give the titled compound (0.100 g).

Aufarbeitung

  1. washThe organic layer was washed with 10% aqueous potassium carbonate and saturated aqueous sodium chloride solution
  2. customdried
  3. concentrationconcentrated
  4. customThe residue was recrystallized

Quellen und Nachweise

ORD-Eintrag
ord-fc5eddb1212c45ee9373ad34bd861204
Quelldatensatz
uspto-grants-2006_10
Patentnummer
US07115750B1

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