Reacción #94951

ord-7766b44aae14420995ee55d945992721

Condiciones de reacción

Temperatura
70°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otrothe reaction
  2. 2
    TemperaturaAfter cooling
  3. 3
    Temperaturaat reflux temperature
  4. 4
    TemperaturaThe reaction mixture is cooled
  5. 5
    ExtracciónThe product is extracted with 2,2'-oxybispropane
  6. 6
    LavadoThe extract is washed with water
  7. 7
    Otrodried
  8. 8
    Filtraciónfiltered
  9. 9
    Otroevaporated

Procedimiento

To 5 parts of magnesium are added 2.18 parts of 1,2-dibromoethane and a small amount of iodine to initiate the reaction. Then there is added dropwise a solution of 28 parts of 4-chloro-1-methylpiperidine in 180 parts of tetrahydrofuran while the mixture is heated to 70° C. After cooling, there is added dropwise a solution of 14 parts of 3-methylbenzonitrile in 90 parts of tetrahydrofuran. Upon completion, stirring is continued for 1 hour at reflux temperature. The reaction mixture is cooled and poured onto a solution of 75 parts of ammonium chloride in water. The product is extracted with 2,2'-oxybispropane. The extract is washed with water, dried, filtered and evaporated, yielding 35 parts of (3-methylphenyl) (1-methyl-4-piperidinyl)methanone as an oily residue.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04342870uspto-grants-1982_08