Piperazine → HCID 54302754, compound

HRID 1608656Notes

Reaction equation

HRID 1608656 reaction equation
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[F:7][C:8]1[CH:13]=[CH:12][C:11]([CH:14]=[CH:15][CH2:16]Cl)=[CH:10][CH:9]=1>C(O)C>[F:7][C:8]1[CH:13]=[CH:12][C:11]([CH:14]=[CH:15][CH2:16][N:1]2[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]2)=[CH:10][CH:9]=1

Participants

4

Reactant 2

HCID 4837PiperazineHCID 536642611-(3-Chloro-1-propen-1-yl)-4-fluorobenzene

Product 1

HCID 54302754HCID 54302754, compoundYield 66.3%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent2×

Procedure

To a boiling solution of 32.4 g (376 mmoles) of anhydrous piperazine in 45 ml of anhydrous ethanol a solution of 6.3 g (37 mmoles) of 3-(4-fluorophenyl)-2-propenyl chloride in 60 ml of anhydrous ethanol is dropped under stirring and reflux cooling, within 1 hour. The solvent is removed in vacuo, the residue is dissolved in chloroform and washed with water to be free from piperazine. The organic phase is dried, evaporated and the crude product is--if necessary--distilled off in vacuo. Thus 5.4 g (66%) of the desired compound are obtained. B.p.: 148° C./80 Pa.

Workup

  1. temperaturereflux
  2. temperaturecooling, within 1 hour
  3. customThe solvent is removed in vacuo
  4. dissolutionthe residue is dissolved in chloroform
  5. washwashed with water
  6. customThe organic phase is dried
  7. customevaporated
  8. distillationif necessary--distilled off in vacuo

Sources & evidence

ORD record
ord-3c9bc28399074cc7a4b638504516353a
Source dataset
uspto-grants-1995_03
Patent number
US05395934

Reaction notes

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