Hydrochloric Acid → HCID 54759636, compound

HRID 473300Notes

Reaction equation

HRID 473300 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]>CC(O)C>[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

4

Reactant 2

HCID 313Hydrochloric Acid2×HCID 46207586Ilorasertib

Product 1

HCID 54759636HCID 54759636, compound

Reagents, catalysts & solvents 1

HCID 3776IsopropanolSolvent2×

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 (126 mg) was suspended in 2-propanol (2.0 mL) at 40° C. with magnetic stirring. Hydrochloric acid (284 μL, 1 N) was diluted with 2-propanol (216 μL). Hydrochloric acid solution was then 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-9c63be86975b4981b5aa991f0806d947
Source dataset
uspto-grants-2014_01
Patent number
US08633317B2

Reaction notes

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