4-[(2,4-Dichloro-5-methoxyphenyl)amino]-6-methoxy-7-[3-(4-methyl-1-piperazinyl)propoxy]-3-quinolinecarbonitrile → HCID 86610056, Verbindung

HRID 499132Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 499132
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([O:9][CH3:10])=[CH:4][C:3]=1[NH:11][C:12]1[C:21]2[C:16](=[CH:17][C:18]([O:24][CH2:25][CH2:26][CH2:27][N:28]3[CH2:33][CH2:32][N:31]([CH3:34])[CH2:30][CH2:29]3)=[C:19]([O:22][CH3:23])[CH:20]=2)[N:15]=[CH:14][C:13]=1[C:35]#[N:36]>C(O)(C)C.O>[CH:5]([O-:9])([CH3:6])[CH3:4].[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([O:9][CH3:10])=[CH:4][C:3]=1[NH:11][C:12]1[C:21]2[C:16](=[CH:17][C:18]([O:24][CH2:25][CH2:26][CH2:27][N:28]3[CH2:33][CH2:32][N:31]([CH3:34])[CH2:30][CH2:29]3)=[C:19]([O:22][CH3:23])[CH:20]=2)[N:15]=[CH:14][C:13]=1[C:35]#[N:36]

Komponenten

3

Edukt 1

HCID 53289404-[(2,4-Dichloro-5-methoxyphenyl)amino]-6-methoxy-7-[3-(4-methyl-1-piperazinyl)propoxy]-3-quinolinecarbonitrile

Produkt 1

HCID 86610056HCID 86610056, VerbindungAusbeute 162,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 21889133Propan-2-ol--water (1/1)Lösungsmittel

Versuchsvorschrift

4-[(2,4-Dichloro-5-methoxyphenyl)amino]-6-methoxy-7-[3-(4-methyl-1-piperazinyl)propoxy]-3-quinolinecarbonitrile (5 g) and 40 mL of a mixture of 2/1 isopropyl alcohol/water (v/v) were added to a 125 flask, and heated to reflux. The mixture was cooled over night to room temperature and filtered. The cake was washed with 15 mL of a 2/1 mixture of isopropyl alcohol/water (v/v) and vacuum dried at 45° C. to give 4.51 g of 4-[(2,4-dichloro-5-methoxyphenyl)amino]-6-methoxy-7-[3-(4-methyl-1-piperazinyl)propoxy]-3-quinolinecarbonitrile monoisopropyl alcoholate as determined by GLC and NMR and determined to be Form III by XRD scans.

Aufarbeitung

  1. temperatureheated to reflux
  2. filtrationfiltered
  3. washThe cake was washed with 15 mL of a 2/1 mixture of isopropyl alcohol/water (v/v) and vacuum
  4. customdried at 45° C.

Quellen und Nachweise

ORD-Eintrag
ord-e321b645f8c8482dbf24be9b981e8f33
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07767678B2

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