Methylamine → HCID 54389278, compound

HRID 1781409Notes

Reaction equation

HRID 1781409 reaction equation
[CH3:1][NH2:2].[C:3]([C:6]1[CH:7]=[C:8]([S:13](Cl)(=[O:15])=[O:14])[CH:9]=[CH:10][C:11]=1[OH:12])(=[O:5])[CH3:4]>C(#N)C>[CH3:1][NH:2][S:13]([C:8]1[CH:9]=[CH:10][C:11]([OH:12])=[C:6]([C:3](=[O:5])[CH3:4])[CH:7]=1)(=[O:15])=[O:14]

Participants

4

Reactant 2

HCID 6329MethylamineHCID 19045468HCID 19045468, compound

Product 1

HCID 54389278HCID 54389278, compound

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

A saturated solution of monomethyl amine in acetonitrile cooled to 0° C. was treated with 3-acetyl-4-hydroxy-benzenesulfonyl chloride. The mixture was stirred 5 min, concentrated .in vacuo to an oil, disolved in ethyl acetate and treated with 1N aqueous HCl. The organic portion was separated, concentrated, filtered through silica gel (eluted with ethyl acetate) to provide N-methyl-3-acetyl-4-hydroxy-benzenesulfonic acid amide after concentration.

Workup

  1. concentrationconcentrated .in vacuo to an oil
  2. additiontreated with 1N aqueous HCl
  3. customThe organic portion was separated
  4. concentrationconcentrated
  5. filtrationfiltered through silica gel (eluted with ethyl acetate)

Sources & evidence

ORD record
ord-fde626f3f44f49ed940d53fb770966eb
Source dataset
uspto-grants-1997_05
Patent number
US05633247

Reaction notes

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