Methanol → HCID 178425952, compound

HRID 1293129Notes

Reaction equation

HRID 1293129 reaction equation
[OH2:1].[CH3:2][C:3]1[CH:8]=[C:7]([CH3:9])[CH:6]=[C:5]([CH3:10])[C:4]=1[S:11][C:12]1[N:16]=[CH:15][NH:14][N:13]=1.C[OH:18]>>[CH3:10][C:5]1[CH:6]=[C:7]([CH3:9])[CH:8]=[C:3]([CH3:2])[C:4]=1[S:11]([C:12]1[N:16]=[CH:15][NH:14][N:13]=1)(=[O:18])=[O:1]

Participants

4

Conditions

Temperature
60 °C

Procedure

A mixture of OXONE monopersulfate compound (50 g) and water (100 ml) was heated on an oil bath at 60° C., to which was added dropwise a mixture of 3-(2,4,6-trimethylphenyl)thio-1H-1,2,4-triazole (Example 32-a) (5.00 g) and methanol (150 ml) over 1 hour with stirring. After the addition was completed, the reaction mixture was heated and refluxed for 3 hours, and then cooled to room temperature and stirred overnight. Precipitated crystals were collected by filtration, and washed with water to yield the title compound (5.03 g).

Workup

  1. additionwas added dropwise
  2. additionAfter the addition
  3. temperaturethe reaction mixture was heated
  4. temperaturerefluxed for 3 hours
  5. temperaturecooled to room temperature
  6. stirringstirred overnight
  7. customPrecipitated crystals
  8. filtrationwere collected by filtration
  9. washwashed with water

Sources & evidence

ORD record
ord-17fdcf2c757047289ac7e30168773545
Source dataset
uspto-grants-2007_07
Patent number
US07238720B2

Reaction notes

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