Réaction #61969

ord-bfd5a02699f14d76aa3eefc852870588

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Extractionthe aqueous phase was extracted with dichloromethane (2×100 mL)
  2. 2
    SéchageThe combined organic extracts were dried (magnesium sulfate)
  3. 3
    Autreevaporated in vacuo
  4. 4
    workup.DISTILLATIONKugelrohr distillation of the residue (5-10 mm Hg, 120° C.)

Mode opératoire

A solution of potassium carbonate (24.9 g) and piperidine (130 mL) in 1:1 ethanol-water (130 mL) was treated with 3-bromopropan-1-ol (25.0 g). The resulting mixture was stirred vigorously for 20 h. Dichloromethane (200 mL) and water (50 mL) were added and the aqueous phase was extracted with dichloromethane (2×100 mL). The combined organic extracts were dried (magnesium sulfate) and evaporated in vacuo. Kugelrohr distillation of the residue (5-10 mm Hg, 120° C.) gave the title compound as a colorless oil (13.9 g).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07429586B2uspto-grants-2008_09