1H-1,2,4-Triazole → HCID 3823094, compound

HRID 1531801Notes

Reaction equation

HRID 1531801 reaction equation
[CH2:1]([O:3][CH2:4]Cl)[CH3:2].[NH:6]1[CH:10]=[N:9][CH:8]=[N:7]1>C1(C)C=CC=CC=1>[CH2:1]([O:3][CH2:4][N:6]1[CH:10]=[N:9][CH:8]=[N:7]1)[CH3:2]

Participants

4

Reactant 2

HCID 92571H-1,2,4-TriazoleHCID 18523Chloromethyl ethyl ether

Product 1

HCID 3823094HCID 3823094, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent2×

Procedure

A solution of chloromethyl ethyl ether (23.5 g) in toluene (300 ml ), was added dropwise, over an hour, to a solution of 1,2,4-triazole (50 g) in toluene (50 ml), and the reaction stirred at room temperature for 18 hours. On cooling, the reaction mixture was evaporated to dryness in vacuo, the residue triturated with dichloromethane, and the resulting suspension filtered. The filtrate was evaporated in vacuo and purified by column chromatography over silica gel (5/95 methanol/dichloromethane) to afford the title compound as a colorless oil, 23.9 g.

Workup

  1. temperatureOn cooling
  2. customthe reaction mixture was evaporated to dryness in vacuo
  3. customthe residue triturated with dichloromethane
  4. filtrationthe resulting suspension filtered
  5. customThe filtrate was evaporated in vacuo
  6. custompurified by column chromatography over silica gel (5/95 methanol/dichloromethane)

Sources & evidence

ORD record
ord-67d82656fc0e497ebabe9202c04b881d
Source dataset
uspto-grants-2001_03
Patent number
US06200978B1

Reaction notes

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