Ethanol → HCID 14624393, compound

HRID 1650768Notes

Reaction equation

HRID 1650768 reaction equation
[C:1]([C:5]1[N:9]=[C:8](SC)[N:7]([C:12]2[C:17]([Cl:18])=[CH:16][C:15]([Cl:19])=[CH:14][C:13]=2[Cl:20])[N:6]=1)([CH3:4])([CH3:3])[CH3:2].[CH2:21](O)C.O[O:25][S:26]([O-:28])=O.[K+]>O>[C:1]([C:5]1[N:9]=[C:8]([S:26]([CH3:21])(=[O:28])=[O:25])[N:7]([C:12]2[C:17]([Cl:18])=[CH:16][C:15]([Cl:19])=[CH:14][C:13]=2[Cl:20])[N:6]=1)([CH3:2])([CH3:3])[CH3:4]

Participants

5

Reactant 3

HCID 702EthanolHCID 14858089HCID 14858089, compoundHCID 23707502Potassium hydroxy sulfite2×

Product 1

HCID 14624393HCID 14624393, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

3.5 g (0.01 mol) of 3-(tert-butyl)-5-methylthio-1-(2,4,6-trichlorophenyl)-1H-1,2,4-triazole was added to 120 ml of 85% ethanol, and 24.6 g (0.04 mol) of Oxone (trade mark) was further added thereto. The mixture was stirred at room temperature for 4 hours. Then, water was added to such an extent that Oxone (as described above) remained in a small amount, and the mixture was extracted with dichloromethane. The dichloromethane layer was dried, and then the solvent was distilled off. The residue was purified by silica gel column chromatography to obtain 3.0 g (yield: 78.9 g) of the desired compound as white powder. Melting point: 179°-180° C.

Workup

  1. additionwas further added
  2. extractionthe mixture was extracted with dichloromethane
  3. dry with materialThe dichloromethane layer was dried
  4. distillationthe solvent was distilled off
  5. customThe residue was purified by silica gel column chromatography

Sources & evidence

ORD record
ord-2924628c6b314f38aa6f089d0155ef49
Source dataset
uspto-grants-1990_05
Patent number
US04925864

Reaction notes

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