Maleic Acid → HCID 54759819, compound

HRID 473306Notes

Reaction equation

HRID 473306 reaction equation
[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:43])(=[O:42])/[CH:37]=[CH:38]\[C:39]([OH:41])=[O:40]>CN(C)C=O>[C:36]([OH:43])(=[O:42])/[CH:37]=[CH:38]\[C:39]([OH:41])=[O:40].[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

Participants

4

Reactant 2

HCID 444266Maleic AcidHCID 46207586Ilorasertib

Product 1

HCID 54759819HCID 54759819, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

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 (27 mg) was suspended in dimethylformamide (125 μL) at 40° C. with magnetic stirring. Maleic acid solution (120 μL, 0.5 M) was then slowly added to A-968660 free base suspension at 50° C. with magnetic stirring. Crystallization was observed upon complete addition of the acid solution. Solid was collected by centrifuge filtration.

Workup

  1. customCrystallization
  2. additionwas observed upon complete addition of the acid solution
  3. filtrationSolid was collected by centrifuge filtration

Sources & evidence

ORD record
ord-af8222dcdc624bc2ae467a60c8081f22
Source dataset
uspto-grants-2014_01
Patent number
US08633317B2

Reaction notes

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