Methanesulfonic Acid → HCID 178446135, compound

HRID 730011Notes

Reaction equation

HRID 730011 reaction equation
[C:1]([C:5]1[NH:6][C:7]([C:25]2[CH:30]=[CH:29][C:28]([F:31])=[CH:27][CH:26]=2)=[C:8]([C:10]2[N:15]=[C:14]3[N:16]([CH2:20][C:21]([CH3:24])([CH3:23])[CH3:22])[C:17]([NH2:19])=[N:18][C:13]3=[CH:12][CH:11]=2)[N:9]=1)([CH3:4])([CH3:3])[CH3:2].[CH3:32][S:33]([OH:36])(=[O:35])=[O:34]>CC(C)=O>[CH3:32][S:33]([OH:36])(=[O:35])=[O:34].[CH3:32][S:33]([OH:36])(=[O:35])=[O:34].[C:1]([C:5]1[NH:6][C:7]([C:25]2[CH:26]=[CH:27][C:28]([F:31])=[CH:29][CH:30]=2)=[C:8]([C:10]2[N:15]=[C:14]3[N:16]([CH2:20][C:21]([CH3:24])([CH3:23])[CH3:22])[C:17]([NH2:19])=[N:18][C:13]3=[CH:12][CH:11]=2)[N:9]=1)([CH3:2])([CH3:3])[CH3:4]

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 178446132HCID 178446132, compound

Product 1

HCID 178446135HCID 178446135, compoundYield 62%

Reagents, catalysts & solvents 1

HCID 180AcetoneSolvent

Procedure

Dissolve 126 mg (0.3 mmol) 5-[2-tert-butyl-5-(4-fluoro-phenyl)-1H-imidazol-4-yl]-3-(2,2-dimethyl-propyl)-3H-imidazo[4,5-b]pyridin-2-ylamine in 2.0 ml acetone. Add 58 mg methanesulfonic acid incrementally. Add seed crystals and filter the resultant precipitate. Air dry to provide 114 mg (62%) of off-white irregular crystals.

Workup

  1. additionAdd seed crystals
  2. filtrationfilter the resultant precipitate
  3. customAir dry

Sources & evidence

ORD record
ord-7b6fc2f7b2734d6b932281f135493898
Source dataset
uspto-grants-2009_09
Patent number
US07582652B2

Reaction notes

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