반응 #67962

ord-1a20acba42b44c2fb88c7da546c2a2e8

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08524738B2uspto-grants-2013_09