Methanesulfonic Acid → HCID 23036496, compound

HRID 1709768Notes

Reaction equation

HRID 1709768 reaction equation
[CH2:1]([O:3][C:4]([CH3:31])([CH3:30])[CH2:5][S:6][CH2:7][C:8]1[C:13]([CH3:14])=[C:12]([O:15][CH3:16])[CH:11]=[CH:10][N+:9]=1[C:17]1[NH:18][C:19]2[CH:25]=[C:24]([C:26]([F:29])([F:28])[F:27])[CH:23]=[CH:22][C:20]=2[N:21]=1)[CH3:2].[CH3:32][S:33]([OH:36])(=[O:35])=[O:34]>CO>[CH3:32][S:33]([O-:36])(=[O:35])=[O:34].[CH2:1]([O:3][C:4]([CH3:30])([CH3:31])[CH2:5][S:6][CH2:7][C:8]1[C:13]([CH3:14])=[C:12]([O:15][CH3:16])[CH:11]=[CH:10][N+:9]=1[C:17]1[NH:18][C:19]2[CH:25]=[C:24]([C:26]([F:28])([F:27])[F:29])[CH:23]=[CH:22][C:20]=2[N:21]=1)[CH3:2]

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 23036497HCID 23036497, compound

Product 1

HCID 23036496HCID 23036496, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

450 mg of intramolecularly deprotonized 2-[((2-ethoxy-2-methylpropyl)thio]methyl]-4-methoxy-3-methyl-1-[5-(trifluoromethyl)-2-benzimidazolyl]pyridinium cation were dissolved in methanol and treated with 110 mg of methanesulfonic acid. The solution was concentrated several times while adding n-hexane each time. The residue was crystallized from tert. butyl methyl ether. The 2-[[(2-ethoxy-2-methylpropyl)thio]methyl]-4-methoxy-3-methyl-1-[5-(trifluoromethyl)-2-benzimidazolyl]pyridinium methanesulfonate obtained exhibited a melting point of 49°-54°.

Workup

  1. concentrationThe solution was concentrated several times
  2. additionwhile adding n-hexane each time
  3. customThe residue was crystallized from tert. butyl methyl ether

Sources & evidence

ORD record
ord-5eae37a5efbc427cb33fee1491633b8e
Source dataset
uspto-grants-1990_08
Patent number
US04950677

Reaction notes

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