Triethylamine → HCID 178522952, Verbindung
Reaktionsgleichung
Cl.Cl.[NH:3]1[C:11]2[CH2:10][CH2:9][NH:8][CH2:7][C:6]=2[N:5]=[CH:4]1.C(N(CC)CC)C.[Cl:19][C:20]1[CH:29]=[C:28]([Cl:30])[CH:27]=[CH:26][C:21]=1[CH2:22][N:23]=[C:24]=[O:25]>C(O)C>[Cl:19][C:20]1[CH:29]=[C:28]([Cl:30])[CH:27]=[CH:26][C:21]=1[CH2:22][NH:23][C:24]([N:8]1[CH2:9][CH2:10][C:11]2[NH:3][CH:4]=[N:5][C:6]=2[CH2:7]1)=[O:25]Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
To a mixture of 4,5,6,7-tetrahydroimidazo[4,5-c]pyridine dihydrochloride (0.50 g, 2.55 mmol), ethanol (10 mL) and triethylamine (1.10 mL, 7.89 mmol), 2,4-dichlorobenzyl isocyanate (0.52 g, 2.57 mmol) was added. The resulting mixture was stirred at room temperature for 16 h and then concentrated under reduced pressure. The residue was distributed between water (20 mL) and ethyl acetate (75 mL). The organic phase was washed with water (10 mL) and brine (10 mL), dried (MgSO4) and concentrated under reduced pressure. The residue was triturated in diethylether (50 mL) and the crude product was filtered off. Recrystallization from acetone (25 mL) gave 0.30 g (37%) of the title urea as a colourless solid.
Aufarbeitung
- additionwas added
- concentrationconcentrated under reduced pressure
- washThe organic phase was washed with water (10 mL) and brine (10 mL)
- dry with materialdried (MgSO4)
- concentrationconcentrated under reduced pressure
- customThe residue was triturated in diethylether (50 mL)
- filtrationthe crude product was filtered off
- customRecrystallization from acetone (25 mL)
Quellen und Nachweise
- ORD-Eintrag
- ord-05512a3be2834b409d2d52b1282b104e
- Quelldatensatz
- uspto-grants-2005_06
- Patentnummer
- US06908926B1
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