Methanesulfonic Acid → HCID 86692568, compound

HRID 1748631Notes

Reaction equation

HRID 1748631 reaction equation
[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[CH3:6][C:7]1[N:11]([C:12]2[CH:17]=[CH:16][C:15]([C:18]([F:21])([F:20])[F:19])=[CH:14][N:13]=2)[N:10]=[CH:9][C:8]=1[C:22]([NH:24][C:25]1[CH:26]=[N:27][C:28]([C:31]2[CH2:36][CH2:35][CH:34]([N:37]3[CH2:42][CH2:41][O:40][CH2:39][CH2:38]3)[CH2:33][CH:32]=2)=[CH:29][CH:30]=1)=[O:23]>C(Cl)(Cl)Cl.CO>[S:2]([OH:5])(=[O:4])(=[O:3])[CH3:1].[CH3:6][C:7]1[N:11]([C:12]2[CH:17]=[CH:16][C:15]([C:18]([F:20])([F:21])[F:19])=[CH:14][N:13]=2)[N:10]=[CH:9][C:8]=1[C:22]([NH:24][C:25]1[CH:26]=[N:27][C:28]([C:31]2[CH2:36][CH2:35][CH:34]([N:37]3[CH2:38][CH2:39][O:40][CH2:41][CH2:42]3)[CH2:33][CH:32]=2)=[CH:29][CH:30]=1)=[O:23]

Participants

5

Reactant 2

HCID 6395Methanesulfonic AcidHCID 86692569HCID 86692569, compound

Product 1

HCID 86692568HCID 86692568, compound

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 6212ChloroformSolvent

Procedure

Methanesulfonic acid (35 μl) was added at room temperature to a solution of 5-methyl-N-{6-[4-(morpholin-4-yl)cyclohex-1-en-1-yl]pyridin-3-yl}-1-[5-(trifluoromethyl)pyridin-2-yl]-1H-pyrazole-4-carboxamide (245 mg) in chloroform (9.0 ml) and methanol (1.0 ml), and stirred at the same temperature for 12 hours. After the reaction, the solvent was evaporated, ethyl acetate was added to the resulting residue and the precipitated solid was filtered to give the titled compound (265 mg) as a white solid.

Workup

  1. customAfter the reaction
  2. customthe solvent was evaporated
  3. additionethyl acetate was added to the resulting residue
  4. filtrationthe precipitated solid was filtered

Sources & evidence

ORD record
ord-428cc97b23204011b027802ea6a7b4a2
Source dataset
uspto-grants-2015_10
Patent number
US09150555B2

Reaction notes

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