Methanesulfonic Acid → HCID 86624481, compound

HRID 557284Notes

Reaction equation

HRID 557284 reaction equation
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[O:7][CH2:8][C:9]1[CH:27]=[CH:26][C:12]([CH2:13][C:14]2[CH:18]=[C:17]([C:19]3[C:20]([NH2:25])=[N:21][CH:22]=[CH:23][CH:24]=3)[O:16][N:15]=2)=[CH:11][CH:10]=1.[CH3:28][S:29]([OH:32])(=[O:31])=[O:30]>CO.C(OCC)(=O)C>[CH3:28][S:29]([OH:32])(=[O:31])=[O:30].[CH3:28][S:29]([OH:32])(=[O:31])=[O:30].[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[O:7][CH2:8][C:9]1[CH:27]=[CH:26][C:12]([CH2:13][C:14]2[CH:18]=[C:17]([C:19]3[C:20]([NH2:25])=[N:21][CH:22]=[CH:23][CH:24]=3)[O:16][N:15]=2)=[CH:11][CH:10]=1

Participants

5

Reactant 2

HCID 6395Methanesulfonic AcidHCID 16719049E-1210

Product 1

HCID 86624481HCID 86624481, compound

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 8857Ethyl AcetateSolvent

Procedure

3-(3-(4-(Pyridin-2-yloxymethyl)-benzyl)-isoxazol-5-yl)-pyridin-2-yl amine (500 mg) was dissolved in methanol (5 mL) and ethyl acetate (5 mL), and methanesulfonic acid (185 μL) was added thereto. The solvent was concentrated under a reduced pressure, to the residue were added ethanol (5 mL) and tert-butyl methyl ether (2 mL), then subjected to ultrasound treatment to be solidified. The solids were filtered to obtain the title compound (630 mg).

Workup

  1. concentrationThe solvent was concentrated under a reduced pressure, to the residue
  2. additionwere added ethanol (5 mL) and tert-butyl methyl ether (2 mL)
  3. filtrationThe solids were filtered

Sources & evidence

ORD record
ord-0ad3e01354c245a780838cfb79695d5f
Source dataset
uspto-grants-2011_11
Patent number
US08058444B2

Reaction notes

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