Potassium Carbonate → 6-(3-Phenoxycarbonylaminopropoxy)carbostyril

HRID 1856766Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1856766
Cl.[NH2:2][CH2:3][CH2:4][CH2:5][O:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][CH:16]=1)[NH:13][C:12](=[O:17])[CH:11]=[CH:10]2.C(=O)([O-])[O-].[K+].[K+].[C:24](Cl)(=[O:32])[O:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1>O.C(#N)C>[O:25]([C:24]([NH:2][CH2:3][CH2:4][CH2:5][O:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][CH:16]=1)[NH:13][C:12](=[O:17])[CH:11]=[CH:10]2)=[O:32])[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1

Komponenten

6

Edukt 3

HCID 11430Potassium CarbonateHCID 15891Phenyl chloroformateHCID 114141486-(3-aminopropoxy)-1H-quinolin-2-one;hydrochloride

Produkt 1

HCID 221326106-(3-Phenoxycarbonylaminopropoxy)carbostyrilAusbeute 90,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel2×HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

To a mixture of water (50 ml) and acetonitrile (50 ml) are added 6-(3-aminopropoxy)carbostyril hydrochloride (5.0 g) and potassium carbonate (3.4 g) at room temperature. The mixture is stirred at room temperature for 2 hours, and cooled to -5° C. To the mixture is added dropwise phenyl chlorocarbonate (3.9 g) while the temperature of the mixture is kept below 0° C. The mixture is stirred at the same temperature for 1 hour, and thereto is added water (100 ml), and then the mixture is further stirred for 0.5 hour. The precipitated crystals are collected by filtration, and washed successively with water and acetone to give 6-(3-phenoxycarbonylaminopropoxy)carbostyril (6.0 g) as a white powder.

Aufarbeitung

  1. temperaturecooled to -5° C
  2. customis kept below 0° C
  3. stirringThe mixture is stirred at the same temperature for 1 hour
  4. stirringthe mixture is further stirred for 0.5 hour
  5. filtrationThe precipitated crystals are collected by filtration
  6. washwashed successively with water and acetone

Quellen und Nachweise

ORD-Eintrag
ord-42764983a41c4be598441f4d5877af9a
Quelldatensatz
uspto-grants-2000_11
Patentnummer
US06143763

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