Hydrochloric Acid → HCID 54759636, compound

HRID 473299Notes

Reaction equation

HRID 473299 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 (27 mg) was suspended in 2-propanol (750 μL) at 40° C. with magnetic stirring. Hydrochloric acid (60 μL, 1 N) was diluted with 2-propanol (250 μL). Hydrochloric acid solution was then slowly added to the 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-248e3573285c42e5934fce54254f96a6
Source dataset
uspto-grants-2014_01
Patent number
US08633317B2

Reaction notes

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