Potassium Carbonate → HCID 178504810, compound

HRID 1869473Notes

Reaction equation

HRID 1869473 reaction equation
[CH3:1][S:2]([C:5]1[CH:14]=[CH:13][C:8]([O:9][CH2:10][C:11]#[N:12])=[CH:7][CH:6]=1)(=[O:4])=[O:3].C([O-])([O-])=O.[K+].[K+].Cl.[NH2:22][OH:23]>O.CCO>[OH:23][NH:22][C:11](=[NH:12])[CH2:10][O:9][C:8]1[CH:7]=[CH:6][C:5]([S:2]([CH3:1])(=[O:3])=[O:4])=[CH:14][CH:13]=1

Participants

6

Procedure

To a mixture of (4-methanesulfonyl-phenoxy)-acetonitrile (2 g, 9.5 mmol), K2CO3 (1.3 g, 9.5 mmol) in H2O (30 mL) and EtOH (15 mL) was added hydroxylamine hydrogen chloride (1.32 g, 19 mmol). The mixture was heated under reflux overnight, cooled and ethanol was removed in vacuo and the residue was extracted with EtOAc (150 mL). The organic layer was washed successively with H2O and brine. After drying (Na2SO4), the solvent was removed to afford the desired product.

Workup

  1. temperatureThe mixture was heated
  2. temperatureunder reflux overnight
  3. temperaturecooled
  4. customethanol was removed in vacuo
  5. extractionthe residue was extracted with EtOAc (150 mL)
  6. washThe organic layer was washed successively with H2O and brine
  7. dry with materialAfter drying (Na2SO4)
  8. customthe solvent was removed

Sources & evidence

ORD record
ord-1d16c30b2483491b88886f74b77d02c0
Source dataset
uspto-grants-2009_12
Patent number
US07638541B2

Reaction notes

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