Réaction #216691

ord-727d90758f5b439798d9429b7630698f

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    workup.ADDITIONwas gradually dropped under ice-
  2. 2
    Températurecooling conditions
  3. 3
    ExtractionThe reaction solution was extracted with chloroform
  4. 4
    Séchagedried with anhydrous magnesium sulfate
  5. 5
    FiltrationThe sulfate was filtered off
  6. 6
    workup.DISTILLATIONthe solvent was distilled off

Mode opératoire

50 g of 4-piperdine ethanol and 49.2 g of sodium hydrogencarbonate were dissolved in 480 ml of water, in which 55.2 ml of benzyloxycarbonyl chloride was gradually dropped under ice-cooling conditions, followed by agitation for 1 hour as it is. The reaction solution was extracted with chloroform and dried with anhydrous magnesium sulfate. The sulfate was filtered off and the solvent was distilled off, after which the resultant residue was subjected to silica gel column chromatography (developing solvent: ethyl acetate:hexane=30:70) to obtain 66.0 g of the captioned compound (yield:65%).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US05468740uspto-grants-1995_11