Hydrogen Peroxide → HCID 20455884, compound

HRID 1262782Notes

Reaction equation

HRID 1262782 reaction equation
[Cl:1][C:2]1[CH:7]=[C:6]([O:8][C:9]2[CH:14]=[C:13]([Cl:15])[C:12]([S:16][CH3:17])=[CH:11][C:10]=2[Cl:18])[CH:5]=[CH:4][N:3]=1.[OH:19]O.O>C(O)(=O)C>[Cl:1][C:2]1[CH:7]=[C:6]([O:8][C:9]2[CH:14]=[C:13]([Cl:15])[C:12]([S:16]([CH3:17])=[O:19])=[CH:11][C:10]=2[Cl:18])[CH:5]=[CH:4][N:3]=1

Participants

5

Reactant 3

HCID 784Hydrogen PeroxideHCID 962WaterHCID 54213038HCID 54213038, compound

Product 1

HCID 20455884HCID 20455884, compound

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Conditions

Temperature
50 °C

Procedure

An amount of 32.6 gm (0.1 mol) of 2-chloro-4-(2,5-dichloro-4-methylmercaptophenoxy)-pyridine, prepared analogously to Example 1, was suspended in 100 ml of glacial acetic acid. The mixture was warmed to 45° to 50° C., and 11 ml (0.11 mol) of 30% H2O2 were added dropwise at such a rate that the internal temperature did not exceed 50° C. The mixture was then stirred for 3 hours at 50° C., after which it was cooled and poured into 300 ml of water. The batch was stirred until crystallization was complete, and the product was recovered by suction filtration, washed with water, dried, and recrystallized from ethyl acetate.

Workup

  1. temperatureThe mixture was warmed to 45° to 50° C.
  2. customdid not exceed 50° C
  3. temperatureafter which it was cooled
  4. stirringThe batch was stirred until crystallization
  5. filtrationthe product was recovered by suction filtration
  6. washwashed with water
  7. customdried
  8. customrecrystallized from ethyl acetate

Sources & evidence

ORD record
ord-7cb7bc1f7c1a4c939fcffcb12178461d
Source dataset
uspto-grants-1984_06
Patent number
US04453972

Reaction notes

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