Dimethyl Sulfoxide → HCID 131727715, Verbindung

HRID 1432154Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1432154
[Cl:1][C:2]1[CH:3]=[C:4]([CH:28]=[CH:29][C:30]=1[F:31])[NH:5][C:6]1[C:15]2[C:10](=[CH:11][C:12]([O:26][CH3:27])=[C:13]([O:16][CH2:17][CH2:18][CH2:19][N:20]3[CH2:25][CH2:24][O:23][CH2:22][CH2:21]3)[CH:14]=2)[N:9]=[CH:8][N:7]=1.[CH3:32][S:33]([CH3:35])=[O:34]>C(OCC)(=O)C>[CH3:27][O:26][C:12]1[CH:11]=[C:10]2[N:9]=[CH:8][N:7]=[C:6]([NH:5][C:4]3[CH:28]=[CH:29][C:30]([F:31])=[C:2]([Cl:1])[CH:3]=3)[C:15]2=[CH:14][C:13]=1[O:16][CH2:17][CH2:18][CH2:19][N:20]1[CH2:25][CH2:24][O:23][CH2:22][CH2:21]1.[CH3:32][S:33]([CH3:35])=[O:34]

Komponenten

4

Edukt 2

HCID 679Dimethyl SulfoxideHCID 123631Gefitinib

Produkt 1

HCID 131727715HCID 131727715, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
75 °C

Versuchsvorschrift

With warming to about 75° C., 4-(3′-chloro-4′-fluoroanilino)-7-methoxy-6-(3-morpholinopropoxy)quinazoline (204 kg) was dissolved in a mixture of ethyl acetate (1021 liters) and dimethyl sulphoxide (181 liters) containing diatomaceous earth filter aid (5 kg). The resultant mixture was filtered and ethyl acetate (78 liters) was used to wash the filter aid solid. The filtrate and washings were combined and cooled initially to about 10° C. The mixture was then heated to about 40° C. for 1 hour. The warm mixture was cooled to 0° C. at a rate of about 10° C. per hour. The resultant solid was collected by filtration. There was thus obtained Form 3 ZD1839 DMSO solvate as shown by XRPD and DSC analysis.

Aufarbeitung

  1. additioncontaining diatomaceous earth
  2. filtrationfilter aid (5 kg)
  3. filtrationThe resultant mixture was filtered
  4. washto wash the filter aid solid
  5. temperaturecooled initially to about 10° C
  6. temperatureThe mixture was then heated to about 40° C. for 1 hour
  7. temperatureThe warm mixture was cooled to 0° C. at a rate of about 10° C. per hour
  8. filtrationThe resultant solid was collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-29301d8c00c240a0985908ab3ea9279a
Quelldatensatz
uspto-grants-2009_11
Patentnummer
US07612077B2

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