반응 #1573972

ord-cb9342a1a0d4402cb5cb96e391e19395

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도heated
  2. 2
    온도under reflux
  3. 3
    여과filtered
  4. 4
    농축concentrated
  5. 5
    기타separated by column chromatography (eluent: dichloromethane/methanol/triethylamine system, v/v/v 100:1:0.5)

실험 절차

Ethyl N-piperazinecarboxylate (25.50 g, 161.39 mmol), 5-bromo-1-pentanol (26.96 g, 161.39 mmol), potassium carbonate (55.68 g, 403.48 mmol) and anhydrous acetonitrile (200 mL) were placed in a 500 mL round-bottomed flask and heated under reflux with stirring overnight; the reaction system was cooled down to room temperature, filtered, concentrated and separated by column chromatography (eluent: dichloromethane/methanol/triethylamine system, v/v/v 100:1:0.5), to obtain a pale yellow oil 20.48 g, yield 52.0% (which was directly used in the next step reaction).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09428496B2uspto-grants-2016_08