Methanesulfonic Acid → HCID 23036534, compound

HRID 1709763Notes

Reaction equation

HRID 1709763 reaction equation
[C:1]([O:4][C:5]([CH3:32])([CH3:31])[CH2:6][S:7][CH2:8][C:9]1[C:14]([CH3:15])=[C:13]([O:16][CH3:17])[CH:12]=[CH:11][N+:10]=1[C:18]1[NH:19][C:20]2[CH:26]=[C:25]([C:27]([F:30])([F:29])[F:28])[CH:24]=[CH:23][C:21]=2[N:22]=1)(=[O:3])[CH3:2].[CH3:33][S:34]([OH:37])(=[O:36])=[O:35]>CO>[CH3:33][S:34]([O-:37])(=[O:36])=[O:35].[C:1]([O:4][C:5]([CH3:32])([CH3:31])[CH2:6][S:7][CH2:8][C:9]1[C:14]([CH3:15])=[C:13]([O:16][CH3:17])[CH:12]=[CH:11][N+:10]=1[C:18]1[NH:19][C:20]2[CH:26]=[C:25]([C:27]([F:29])([F:30])[F:28])[CH:24]=[CH:23][C:21]=2[N:22]=1)(=[O:3])[CH3:2]

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 23036532HCID 23036532, compound

Product 1

HCID 23036534HCID 23036534, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

467.5 mg of intramolecularly deprotonized 2-[[(2-acetoxy-2-methylpropyl)thio]methyl]-4-methoxy-3 methyl-1-[5-(trifluoromethyl)-2-benzimidazolyl]pyridinium cation were dissolved in 5 ml of methanol, whereupon 96 mg of methanesulfonic acid were added thereto, the solution was concentrated, the residue was dissolved several times in ethyl acetate and the solution was again concentrated each time. The resinous residue was dried in a high vacuum, whereby 2-[[(2-acetoxy-2-methylpropyl)thio]methyl]-4-methoxy-3-methyl-1-[5-(trifluoromethyl)-2-benzimidazolyl]pyridinium methanesulfonate (1:1) was obtained as a foam. The microanalysis showed the following values:

Workup

  1. additionwere added
  2. concentrationthe solution was concentrated
  3. dissolutionthe residue was dissolved several times in ethyl acetate
  4. concentrationthe solution was again concentrated each time
  5. customThe resinous residue was dried in a high vacuum

Sources & evidence

ORD record
ord-b91fe44cd6394a6eb3b2f38a923151be
Source dataset
uspto-grants-1990_08
Patent number
US04950677

Reaction notes

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