Potassium hydroxy sulfite → HCID 68514318, compound

HRID 1717234Notes

Reaction equation

HRID 1717234 reaction equation
[CH:1]1([NH:4][C:5]([C:7]2[N:8]=[N:9][N:10]([C:15]3[CH:20]=[CH:19][C:18]([NH:21][C:22](=[O:27])[CH2:23][CH2:24][S:25][CH3:26])=[CH:17][CH:16]=3)[C:11]=2[CH2:12][CH2:13][CH3:14])=[O:6])[CH2:3][CH2:2]1.[OH:28]OS([O-])=O.[K+]>CO>[CH:1]1([NH:4][C:5]([C:7]2[N:8]=[N:9][N:10]([C:15]3[CH:16]=[CH:17][C:18]([NH:21][C:22](=[O:27])[CH2:23][CH2:24][S:25]([CH3:26])=[O:28])=[CH:19][CH:20]=3)[C:11]=2[CH2:12][CH2:13][CH3:14])=[O:6])[CH2:2][CH2:3]1

Participants

4

Reactant 2

HCID 23707502Potassium hydroxy sulfiteHCID 68514369HCID 68514369, compound

Product 1

HCID 68514318HCID 68514318, compoundYield 86.4%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a solution of N-cyclopropyl-1-(4-{[3-(methylthio)propanoyl]amino}phenyl)-5-propyl-1H-1,2,3-triazole-4-carboxamide (0.10 g) obtained in Example 10 in methanol (6 ml) was added an aqueous solution (2 ml) of Oxone (0.10 g) at room temperature, and the mixture was stirred for 1 hr. The solvent was evaporated under reduced pressure, and the residue was diluted with ethyl acetate and washed with saturated brine. The organic layer was dried over magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was recrystallized from methanol-diethyl ether to give the title compound as a white powder (0.09 g, 82%).

Workup

  1. customThe solvent was evaporated under reduced pressure
  2. additionthe residue was diluted with ethyl acetate
  3. washwashed with saturated brine
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. customthe solvent was evaporated under reduced pressure
  6. customThe residue was recrystallized from methanol-diethyl ether

Sources & evidence

ORD record
ord-32e52a69c68544369f715cf195c47c30
Source dataset
uspto-grants-2010_09
Patent number
US07803822B2

Reaction notes

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