Hydrogen Peroxide → HCID 68526433, compound

HRID 1907653Notes

Reaction equation

HRID 1907653 reaction equation
[CH3:1][N:2]1[C:7](=[O:8])[CH:6]=[C:5]([C:9]2[CH:14]=[CH:13][N:12]=[CH:11][N:10]=2)[N:4]=[C:3]1[CH3:15].S(=O)(=O)(O)O.[I-:21].OO.[Cl-].[NH4+]>O.C(Cl)(Cl)Cl.C(Cl)(Cl)(Cl)Cl>[I:21][CH2:15][C:3]1[N:2]([CH3:1])[C:7](=[O:8])[CH:6]=[C:5]([C:9]2[CH:14]=[CH:13][N:12]=[CH:11][N:10]=2)[N:4]=1

Participants

9

Reactant 5

HCID 784Hydrogen PeroxideHCID 1118Sulfuric AcidHCID 25517Ammonium ChlorideHCID 30165Iodide IonHCID 66613233HCID 66613233, compound

Product 1

HCID 68526433HCID 68526433, compoundYield 112%

Reagents, catalysts & solvents 3

HCID 962WaterSolventHCID 5943Carbon TetrachlorideSolventHCID 6212ChloroformSolvent

Procedure

To a suspension of 17 g (0.084 mol) of 1,2-Dimethyl-1H-[4,4]bipyrimidinyl-6-one in 45 mL of water, were added 8.5 mL of sulfuric acid, 25 mL of carbon tetrachloride and 9.6 g (0.037 mol) of iodide. The resulting mixture was refluxed and 16.38 mL of hydrogen peroxide (35% solution in water) was added dropwise. The mixture was stirred under reflux for 5 h and cooled at room temperature, 100 mL of saturated aqueous solution of ammonium chloride and 100 mL of chloroform were added. The resulting precipitate was filtered off, the filtrate extracted with chloroform, dried and evaporated to afford 13.6 g of product witch was used as such in the next step.

Workup

  1. temperatureThe resulting mixture was refluxed
  2. temperatureunder reflux for 5 h
  3. filtrationThe resulting precipitate was filtered off
  4. extractionthe filtrate extracted with chloroform
  5. customdried
  6. customevaporated

Sources & evidence

ORD record
ord-d69a7229719046ecb7230e1808d2de95
Source dataset
uspto-grants-2013_12
Patent number
US08598175B2

Reaction notes

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