Reacción #64956

ord-43ddd1ffd6604e6ba16a65311fcdf3d1

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturathe mixture is heated
  2. 2
    Temperaturaunder reflux at the same time
  3. 3
    Temperaturathe mixture is then heated
  4. 4
    Temperaturaunder reflux overnight
  5. 5
    Extracciónextracted with toluene
  6. 6
    Secadothe extracts are dried with K2CO3
  7. 7
    Concentraciónconcentrated
  8. 8
    workup.DISTILLATIONthe residue is distilled

Procedimiento

17.3 g (58 mmol) of crude trans-1-benzyl-3-benzylmethylamino-4-hydroxy-pyrrolidine in 80 ml of absolute tetrahydrofuran are added dropwise to 2.8 g (93.3 mmol) of 80% strength sodium hydride in 40 ml of absolute tetrahydrofuran and the mixture is heated under reflux at the same time. When the evolution of hydrogen has ended, 8.7 g (61 mmol) of methyl iodide are added dropwise and the mixture is then heated under reflux overnight. It is poured into ice-water and extracted with toluene, the extracts are dried with K2CO3 and concentrated and the residue is distilled.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05416096uspto-grants-1995_05