Methanesulfonic Acid → HCID 54759637, compound

HRID 473304Notes

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.[CH3:36][S:37]([OH:40])(=[O:39])=[O:38]>C(OCC)(=O)C>[S:37]([OH:40])(=[O:39])(=[O:38])[CH3:36].[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

Conditions

Temperature: 40 °C

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 (71 mg) was suspended in ethyl acetate (1.0 mL) at 45° C. with magnetic stirring. Methanesulfonic acid (36 μL, 4 M) was slowly added to A-968660 free base suspension at 40° C. with magnetic stirring. Amorphous material precipitated upon addition of the acid solution. The suspension was stirred at 40° C. overnight. Solid was collected by centrifuge filtration.

Workup

customAmorphous material precipitated upon addition of the acid solution
filtrationSolid was collected by centrifuge filtration

Sources & evidence

ORD record: ord-e564997ad6b14dd790d45fb48814d506
Source dataset: uspto-grants-2014_01
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US08633317B2

Reaction notes

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