Hydrogen Peroxide → HCID 11043886, compound

HRID 1385511Notes

Reaction equation

HRID 1385511 reaction equation
[OH:1]O.[Cl:3][C:4]1[C:5]([S:14][CH2:15][CH2:16][CH3:17])=[N:6][CH:7]=[C:8]([C:10]([F:13])([F:12])[F:11])[CH:9]=1>C(O)(=O)C>[Cl:3][C:4]1[C:5]([S:14]([CH2:15][CH2:16][CH3:17])=[O:1])=[N:6][CH:7]=[C:8]([C:10]([F:11])([F:12])[F:13])[CH:9]=1

Participants

4

Reactant 2

HCID 784Hydrogen PeroxideHCID 10999654HCID 10999654, compound

Product 1

HCID 11043886HCID 11043886, compound

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Conditions

Temperature
25 °C

Procedure

8.4 g (0.124 mol) of 50% strength hydrogen peroxide were added with stirring at 15-20° C. in the course of 15 minutes to a mixture of 31 g (0.1213 mol) of 3-chloro-2-n-propylthio-5-trifluoromethylpyridine in 150 ml of acetic acid, during which process the temperature rose to 27° C. in the course of 6 hours. After the reaction mixture had been stirred for 14 hours at 25° C., it was poured into ice-water and extracted 3 times with methylene chloride. The organic phase was washed with water and saturated sodium hydrogen carbonate solution, dried and concentrated in vacuo, yielding 32 g (97.2% of theory) of the title compound of m.p. 51-53° C.

Workup

  1. customrose to 27° C. in the course of 6 hours
  2. extractionextracted 3 times with methylene chloride
  3. washThe organic phase was washed with water and saturated sodium hydrogen carbonate solution
  4. customdried
  5. concentrationconcentrated in vacuo

Sources & evidence

ORD record
ord-6f83f47bf4744311af843a51ee143c99
Source dataset
uspto-grants-2001_07
Patent number
US06262273B1

Reaction notes

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