Reacción #65040

ord-fa353175c04246a7aadabf201b983965

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturawas heated
  2. 2
    Temperaturaunder reflux for 2 hours
  3. 3
    Lavadothe mixture was washed successively with water
  4. 4
    Secadoa saturated sodium chloride aqueous solution, and dried over magnesium sulfate
  5. 5
    OtroThe solvent was evaporated under reduced pressure
  6. 6
    workup.ADDITIONa 1:2 mixture of ethyl acetate and hexane as a developing solvent

Procedimiento

A mixture of 6.56 g of 1,12-dibromododecane, 3.24 g of N-phenylpiperazine, 2.53 g of triethylamine, and 50 ml of toluene was heated under reflux for 2 hours. To the reaction mixture was added 100 ml of ethyl acetate, and the mixture was washed successively with water and a saturated sodium chloride aqueous solution, and dried over magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was subjected to column chromatography using a 1:2 mixture of ethyl acetate and hexane as a developing solvent to yield 4.1 g of 1-bromo-12-(4-phenylpiperazinyl)dodecane (m.p.=26.0°-28.0° C.).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05416212uspto-grants-1995_05