Hydrogen Peroxide → HCID 131729532, compound

HRID 1619077Notes

Reaction equation

HRID 1619077 reaction equation
[Br:1][C:2]1[CH:3]=[C:4]([C:14](=[O:33])[CH2:15][C:16]2[C:30]([CH3:31])=[CH:29][C:28]([Cl:32])=[CH:27][C:17]=2[C:18]([N:20]=[S:21]2[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]2)=[O:19])[N:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[Cl:13])[N:6]=1.OO.C(=O)([O-])[O-:37].[Na+].[Na+].C(Cl)Cl>C(O)(=O)C>[Br:1][C:2]1[CH:3]=[C:4]([C:14](=[O:33])[CH2:15][C:16]2[C:30]([CH3:31])=[CH:29][C:28]([Cl:32])=[CH:27][C:17]=2[C:18]([N:20]=[S:21]2(=[O:37])[CH2:22][CH2:23][CH2:24][CH2:25][CH2:26]2)=[O:19])[N:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[Cl:13])[N:6]=1

Participants

6

Reactant 4

HCID 784Hydrogen PeroxideHCID 6344DichloromethaneHCID 10340Sodium CarbonateHCID 131729533HCID 131729533, compound

Product 1

HCID 131729532HCID 131729532, compound

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

0.2 g 2-{2-[5-Bromo-2-(2-chloro-phenyl)-2H-pyrazol-3-yl]-2-oxo-ethyl}-5-chloro-3-methyl-N-(tetrahydro-1 lambda*4*-thiopyran-1-ylidene)-benzamide (0.35 mmol) were dissolved in 10 ml acetic acid. 4 mg Sodium wolframate dihydrate were added. 45 mg of a 30% solution of hydrogenperoxide was added dropwise and the resulting solution was stirred for 18 h. The reaction mixture was poured into a saturated aqueous sodium carbonate solution, methylene chloride was added and the organic pase was subsequently washed with water and saturated aqueous sodium carbonate. The organic solvent was dried and the solvent removed. Column chromatography yielded 0.07 g of the desired product, compound I.4-22.

Workup

  1. additionwas added
  2. washthe organic pase was subsequently washed with water and saturated aqueous sodium carbonate
  3. customThe organic solvent was dried
  4. customthe solvent removed

Sources & evidence

ORD record
ord-b141693fa2164a79b73e002a01340b2c
Source dataset
uspto-grants-2014_07
Patent number
US08772289B2

Reaction notes

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