Dimethyl Sulfate → HCID 54044700, compound

HRID 2397874Notes

Reaction equation

HRID 2397874 reaction equation
[C:1]([NH:4][N:5]1[CH:9]=[N:8][N:7]=[C:6]1[N:10]([C:21](=[O:23])[CH3:22])[N:11]=[CH:12][C:13]1[C:18]([Cl:19])=[CH:17][CH:16]=[CH:15][C:14]=1[Cl:20])(=[O:3])[CH3:2].[C:24](=O)([O-])[O-].[Na+].[Na+].S(OC)(OC)(=O)=O>O>[CH3:24][N:4]([N:5]1[CH:9]=[N:8][N:7]=[C:6]1[N:10]([C:21](=[O:23])[CH3:22])[N:11]=[CH:12][C:13]1[C:14]([Cl:20])=[CH:15][CH:16]=[CH:17][C:18]=1[Cl:19])[C:1](=[O:3])[CH3:2]

Participants

5

Reactant 3

HCID 6497Dimethyl SulfateHCID 10340Sodium CarbonateHCID 4776242HCID 4776242, compound

Product 1

HCID 54044700HCID 54044700, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

To a solution of 31.5 g of 4-acetamido-3[1-acetyl-2-(2,6-dichlorobenzylidene)hydrazino] -1,2,4-triazole and 53.0 g of sodium carbonate in 400 ml of water is added dropwise, while stirring and cooling in an ice bath, 40 ml of dimethyl sulphate (2 h). After the addition the mixture was stirred for 2,5 h while cooling in ice and left overnight at room temperature. The obtained precipitate is collected and recrystallized twice from dioxane-isopropyl ether. Yield: 7.3 g, m.p. 167°-169° .

Workup

  1. temperaturecooling in an ice bath
  2. additionAfter the addition the mixture
  3. stirringwas stirred for 2,5 h
  4. temperaturewhile cooling in ice
  5. customThe obtained precipitate is collected
  6. customrecrystallized twice from dioxane-isopropyl ether

Sources & evidence

ORD record
ord-d4e9fa82b8514c95b77db237a883b7b0
Source dataset
uspto-grants-1977_05
Patent number
US04022905

Reaction notes

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