Phosphorus oxychloride → HCID 21331105, compound

HRID 1729663Notes

Reaction equation

HRID 1729663 reaction equation
[CH2:1]([N:8]1[C:12](O)=[C:11]([CH2:14][CH2:15][C:16]([O:18][CH2:19][CH3:20])=[O:17])[N:10]=[N:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.P(Cl)(Cl)([Cl:23])=O.P(Cl)(Cl)(Cl)(Cl)Cl>>[CH2:1]([N:8]1[C:12]([Cl:23])=[C:11]([CH2:14][CH2:15][C:16]([O:18][CH2:19][CH3:20])=[O:17])[N:10]=[N:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Participants

4

Reactant 3

HCID 24813Phosphorus oxychlorideHCID 24819Phosphorus pentachlorideHCID 178471188HCID 178471188, compound

Product 1

HCID 21331105HCID 21331105, compound

Procedure

To a solution of 1.0 g. (4 mmol.) of 1-benzyl-4-(2-carbethoxyethyl)-5-hydroxy-1,2,3-triazole in 2 ml. of phosphorus oxychloride is added 0.5 g. (5 mmol.) of phosphorus pentachloride. The reaction mixture is stirred at 25° for 2 hours, then warmed on a steam bath for 10 minutes and evaporated to dryness. The residue is dissolved in 0.5 ml. of phosphorus oxychloride and the solution is heated to reflux for 30 minutes, cooled and evaporated to dryness to give 1-benzyl-4-(2-carbethoxyethyl)-5-chloro-1,2,3-triazole.

Workup

  1. temperaturewarmed on a steam bath for 10 minutes
  2. customevaporated to dryness
  3. dissolutionThe residue is dissolved in 0.5 ml
  4. temperatureof phosphorus oxychloride and the solution is heated
  5. temperatureto reflux for 30 minutes
  6. temperaturecooled
  7. customevaporated to dryness

Sources & evidence

ORD record
ord-7d4a8c6d63cd4941a37954a80926c195
Source dataset
uspto-grants-1976_11
Patent number
US03989694

Reaction notes

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