Réaction #67962

ord-1a20acba42b44c2fb88c7da546c2a2e8

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Autrethe solvent was removed under reduced pressure
  2. 2
    AutreThe residue thus obtained
  3. 3
    AutreThe aqueous layer was separated
  4. 4
    workup.ADDITIONethyl acetate was added
  5. 5
    AutreThe organic layer was separated
  6. 6
    Séchagedried over potassium carbonate
  7. 7
    Autrethe solvent was removed under reduced pressure

Mode opératoire

To 0.60 g of 1-tert-butyl 3-ethyl 4-(2-(2,3-dihydro-1,4-benzodioxin-6-yl)ethyl)piperazine-1,3-dicarboxylate, 12 mL of 10 mol/L hydrogen chloride/ethanol was added, and the mixture was stirred for 2 hours, and then the solvent was removed under reduced pressure. The residue thus obtained was added with water and ethyl acetate. The aqueous layer was separated, ethyl acetate was added thereto, and the resultant solution was adjusted to pH 14 with a 5 mol/L aqueous sodium hydroxide solution. The organic layer was separated and dried over potassium carbonate, and the solvent was removed under reduced pressure to obtain 0.34 g of a brown oily substance, ethyl 1-(2-(2,3-dihydro-1,4-benzodioxin-6-yl)ethyl)piperazine-2-carboxylate.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08524738B2uspto-grants-2013_09