Hydrogen Peroxide → HCID 11043886, compound

HRID 636066Notes

Reaction equation

HRID 636066 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
27 °C

Procedure

At 15-20° C., 8.4 g (0.124 mol) of 50% strength hydrogen peroxide were added over a period of 15 min with stirring to a mixture of 31 g (0.1213 mol) of 3-chloro-2-n-propylthio-5-trifluoromethylpyridine in 150 ml of acetic acid, the temperature increasing to 27° C. over a period of 6 h. The reaction mixture was stirred at 25° C. for 14 h and then poured into ice-water and extracted 3 times with methylene chloride. The organic phase was washed with water and saturated sodium bicarbonate solution, dried and concentrated under reduced pressure, giving 32 g (97.2% of theory) of the title compound of mp. 51-53° C.

Workup

  1. extractionextracted 3 times with methylene chloride
  2. washThe organic phase was washed with water and saturated sodium bicarbonate solution
  3. customdried
  4. concentrationconcentrated under reduced pressure

Sources & evidence

ORD record
ord-e21b7f41eb144b62ad9f421a94a5a0c5
Source dataset
uspto-grants-2001_02
Patent number
US06191280B1

Reaction notes

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