Reacción #2396543

ord-3b2ba216faf0424d86d8dc22eda36a71

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturaunder reflux for 5 hours
  2. 2
    TemperaturaAfter cooling
  3. 3
    LavadoThe solution is washed twice with 100 ml of water
  4. 4
    Secadosaturated aqueous solution of sodium chloride, and dried over anhydrous sodium sulfate
  5. 5
    workup.DISTILLATIONAfter distilling off
  6. 6
    Otrochloroform, crystallization from diethylether/methanol

Procedimiento

In 6 ml of methylethylketone, 2.03 g of 6-methyl-4-phenyl-2-piperazinyl-thieno[2,3-d]pyrimidine, 1.25 g of 4-fluorophenacyl chloride and 0.73 g of triethylamine are reacted under reflux for 5 hours. After cooling, 70 ml of chloroform is added to the reaction mixture. The solution is washed twice with 100 ml of water and then saturated aqueous solution of sodium chloride, and dried over anhydrous sodium sulfate. After distilling off chloroform, crystallization from diethylether/methanol gives 2.68 g of the product which has a melting point of 141°-142° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04695568uspto-grants-1987_09