1H-1,2,4-Triazole → HCID 13295575, compound

HRID 1731316Notes

Reaction equation

HRID 1731316 reaction equation
Cl[CH2:2][C:3]([CH2:5]Cl)=[CH2:4].[NH:7]1[CH:11]=[N:10][CH:9]=[N:8]1.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[N:7]1([CH2:2][C:3]([CH2:5][N:7]2[CH:11]=[N:10][CH:9]=[N:8]2)=[CH2:4])[CH:11]=[N:10][CH:9]=[N:8]1

Participants

5

Reactant 3

HCID 92571H-1,2,4-TriazoleHCID 11430Potassium CarbonateHCID 158593-Chloro-2-chloromethyl-1-propene

Product 1

HCID 13295575HCID 13295575, compoundYield 63%

Reagents, catalysts & solvents 1

HCID 180AcetoneSolvent

Procedure

A mixture of 25 g (0.2 mol) of 3-chloro-2-chloromethyl-propene, 27.6 g (0.4 mol) of 1,2,4-triazole and 27.6 g (0.2 mol) of potassium carbonate in 200 ml of acetone is heated under reflux for 15 hours. After cooling, the mixture is filtered and the filtrate is concentrated in vacuo. The oily residue is chromatographed (silica gel 60, Merck, chloroform). 23 g (63% of theory) of 3-(1,2,4-triazol-1-yl)-2-(1,2,4-triazol-1-yl-methyl)-propene of melting point 52° C. are obtained.

Workup

  1. temperatureis heated
  2. temperatureunder reflux for 15 hours
  3. temperatureAfter cooling
  4. filtrationthe mixture is filtered
  5. concentrationthe filtrate is concentrated in vacuo
  6. customThe oily residue is chromatographed (silica gel 60, Merck, chloroform)

Sources & evidence

ORD record
ord-4093ae2d2a4b47e59b743f3f3a06274d
Source dataset
uspto-grants-1986_11
Patent number
US04621095

Reaction notes

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