Hydrochloric Acid → HCID 54759636, compound

HRID 473301Notes

Reaction equation

HRID 473301 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.[ClH:36]>C(O)C.O>[ClH:36].[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

5

Reactant 2

HCID 313Hydrochloric Acid2×HCID 46207586Ilorasertib

Product 1

HCID 54759636HCID 54759636, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent

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 (89 mg) was suspended in ethanol (2.5 mL) at 40° C. with magnetic stirring. Hydrochloric acid (380 μL, 1 N) was diluted with water (620 μL). Hydrochloric acid solution was slowly added to A-968660 free base suspension at 40° C. with magnetic stirring. Crystallization was observed shortly after the complete addition of the HCl solution. Solid was collected by centrifuge filtration.

Workup

  1. customCrystallization
  2. additionafter the complete addition of the HCl solution
  3. filtrationSolid was collected by centrifuge filtration

Sources & evidence

ORD record
ord-a3aad5525ea0495b8596596527c2992a
Source dataset
uspto-grants-2014_01
Patent number
US08633317B2

Reaction notes

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