Methanesulfonic Acid → HCID 13178432, compound

HRID 1981411Notes

Reaction equation

HRID 1981411 reaction equation
CS([O:5][C:6]1[CH:11]=[CH:10][C:9]([C:12](=[NH:14])[NH2:13])=[CH:8][C:7]=1[N+:15]([O-:17])=[O:16])(=O)=O.CS(O)(=O)=O.[C:23](OC(=O)C)(=[O:25])[CH3:24]>>[C:23]([O:5][C:6]1[CH:11]=[CH:10][C:9]([C:12](=[NH:14])[NH2:13])=[CH:8][C:7]=1[N+:15]([O-:17])=[O:16])(=[O:25])[CH3:24]

Participants

4

Reactant 3

HCID 6395Methanesulfonic AcidHCID 7918Acetic AnhydrideHCID 53945002HCID 53945002, compound

Product 1

HCID 13178432HCID 13178432, compound

Procedure

To a suspension of 3.0 g of 4-amidino-2-nitrophenol methanesulfonate in 15 ml of acetic anhydride, was added 0.5 ml of methanesulfonic acid. The mixture was refluxed with stirring for 10 to 20 minutes. The crystals dissolved slowly, forming a clear yellow solution. Upon standing at room temperature, colorless crystals separated out of the solution. The crystals were ashed with ethyl ether and recrystallized from ethanol to obtain 3.0 g of colorless needle crystals of 4-amidino-2-nitrophenyl acetate methanesulfonate.

Workup

  1. temperatureThe mixture was refluxed
  2. dissolutionThe crystals dissolved slowly
  3. customforming a clear yellow solution
  4. customUpon standing at room temperature
  5. customcolorless crystals separated out of the solution
  6. customrecrystallized from ethanol

Sources & evidence

ORD record
ord-4e9056fd1b2f4e379d8646e78cb1aa00
Source dataset
uspto-grants-1985_04
Patent number
US04514416

Reaction notes

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