Methanol → HCID 12877063, compound

HRID 1154733Notes

Reaction equation

HRID 1154733 reaction equation
CO.[CH3:3][C:4]1[N:8]([C:9]2[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[CH:11][CH:10]=2)[N:7]=[C:6]([SH:18])[N:5]=1.[OH-].[Na+].S(OC)(O[CH3:25])(=O)=O>O>[CH3:3][C:4]1[N:8]([C:9]2[CH:10]=[CH:11][C:12]([N+:15]([O-:17])=[O:16])=[CH:13][CH:14]=2)[N:7]=[C:6]([S:18][CH3:25])[N:5]=1

Participants

6

Reactant 4

HCID 887MethanolHCID 6497Dimethyl SulfateHCID 14798Sodium HydroxideHCID 178433555HCID 178433555, compound

Product 1

HCID 12877063HCID 12877063, compoundYield 66%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

To 80 parts of methanol are added 4.7 parts of 5-methyl-1-(4-nitrophenyl)-1H-1,2,4-triazole-3-thiol and 1.2 parts of sodium hydroxide and the whole is stirred till all solid enters solution. Then there are added 2.66 parts of dimethyl sulfate and stirring is continued for 1 hour at room temperature. 100 Parts of water are added. The precipitated product is filtered off, washed with water, dried, and crystallized from 2,2'-oxybispropane, yielding 3.3 parts (66%) of 5-methyl-3-(methylthio)-1-(4-nitrophenyl)-1H-1,2,4-triazole; mp. 121°-125° C.

Workup

  1. stirringstirring
  2. filtrationThe precipitated product is filtered off
  3. washwashed with water
  4. customdried
  5. customcrystallized from 2,2'-oxybispropane

Sources & evidence

ORD record
ord-2262f884be054effb095e8cb4bff6eed
Source dataset
uspto-grants-1984_12
Patent number
US04490530

Reaction notes

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