Reacción #8734

ord-96ec3a24686b406a85e6ce4079bf506b

Ecuación de reacción

NCc1cccc(F)c1
3-fluorobenzylamine
OCCCl
2-chloroethanol
[Na+].[OH-]
sodium hydroxide
OCCNCc1cccc(F)c1
2-(3-fluoro-benzylamino)-ethanol

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Extracciónextract the two-phase mixture twice with 25 mL and 13 mL portions of benzene
  2. 2
    Otroremove the water by co-distillation with benzene through a modified Claisen flask
  3. 3
    workup.DISTILLATIONThe final desired compound may be purified with further distillation

Procedimiento

Combine 3-fluorobenzylamine (31.1 g, 0.248 mol), 2-chloroethanol (10 g, 0.124 mol) and water (30 g, 1.66 mol) and heat on a steam-bath for ˜5 hours. Add sodium hydroxide (15 g, 0.373 mol) to the cooled solution and heat the resulting mixture on a steam-bath for ˜30 minutes. Add water (˜50 mL) to dissolve the inorganic salts and extract the two-phase mixture twice with 25 mL and 13 mL portions of benzene. Combine the extracts and remove the water by co-distillation with benzene through a modified Claisen flask. The final desired compound may be purified with further distillation.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07091199B1uspto-grants-2006_08