Methanol → HCID 178425952, compound
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
- additionwas added dropwise
- additionAfter the addition
- temperaturethe reaction mixture was heated
- temperaturerefluxed for 3 hours
- temperaturecooled to room temperature
- stirringstirred overnight
- customPrecipitated crystals
- filtrationwere collected by filtration
- washwashed with water
Sources & evidence
- ORD record
- ord-17fdcf2c757047289ac7e30168773545
- Source dataset
- uspto-grants-2007_07
- Patent number
- US07238720B2
Reaction notes
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