Citric Acid → HCID 54767922, Verbindung

HRID 472772Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 472772
[NH2:1][C:2]1[C:7]2[C:8]([C:11]3[CH:16]=[CH:15][C:14]([NH:17][C:18]([NH:20][C:21]4[CH:26]=[CH:25][CH:24]=[C:23]([F:27])[CH:22]=4)=[O:19])=[CH:13][CH:12]=3)=[CH:9][S:10][C:6]=2[C:5]([C:28]2[CH:29]=[N:30][N:31]([CH2:33][CH2:34][OH:35])[CH:32]=2)=[CH:4][N:3]=1.[C:36]([OH:48])(=[O:47])[CH2:37][C:38]([CH2:43][C:44]([OH:46])=[O:45])([C:40]([OH:42])=[O:41])[OH:39].CCCCCCC>C1COCC1.O>[C:36]([OH:48])(=[O:47])[CH2:37][C:38]([CH2:43][C:44]([OH:46])=[O:45])([C:40]([OH:42])=[O:41])[OH:39].[NH2:1][C:2]1[C:7]2[C:8]([C:11]3[CH:12]=[CH:13][C:14]([NH:17][C:18]([NH:20][C:21]4[CH:26]=[CH:25][CH:24]=[C:23]([F:27])[CH:22]=4)=[O:19])=[CH:15][CH:16]=3)=[CH:9][S:10][C:6]=2[C:5]([C:28]2[CH:29]=[N:30][N:31]([CH2:33][CH2:34][OH:35])[CH:32]=2)=[CH:4][N:3]=1

Komponenten

5

Edukt 3

HCID 311Citric AcidHCID 8900Heptane2×HCID 46207586Ilorasertib

Produkt 1

HCID 54767922HCID 54767922, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 21881883Oxolane--water (1/1)Lösungsmittel2×

Versuchsvorschrift

N-(4-{4-amino-7-[1-(2-hydroxyethyl)-1H-pyrazol-4-yl]thieno[3,2-c]pyridin-3-yl}phenyl)-N′-(3-fluorophenyl)urea free base solid (102.65 mg) was dissolved in 5 mL of THF/water mixture (80/20 v/v) at 70° C. Citric acid (21.94 mg) was added to the solution followed by the slow addition of heptane (7.5 mL). The appearance of a small amount of precipitant formed in the heptane layer was noted. The precipitant dissolved as it fell into the THF/water layer. The solution was cooled to ambient temperatures. Crystalline solids formed after several days at ambient temperatures. Solid was collected by vacuum filtration.

Aufarbeitung

  1. dissolutionThe precipitant dissolved as it
  2. temperatureThe solution was cooled to ambient temperatures
  3. customCrystalline solids formed after several days at ambient temperatures
  4. filtrationSolid was collected by vacuum filtration

Quellen und Nachweise

ORD-Eintrag
ord-936710ba4eb84f27b3009a94c5a42370
Quelldatensatz
uspto-grants-2014_01
Patentnummer
US08633217B2

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