반응 #51047

ord-8cae2a34954640a9b6a0abd424a54f32

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도heated
  2. 2
    온도to reflux for 20 hours
  3. 3
    여과filtered
  4. 4
    기타The filtrate was evaporated
  5. 5
    기타the residue was triturated under diethyl ether
  6. 6
    여과The resultant mixture was filtered
  7. 7
    기타the filtrate was evaporated
  8. 8
    workup.DISTILLATIONThe residue was purified by distillation at about 60-70° C. under about 0.2 mm Hg

실험 절차

A mixture of 3-bromopropanol (20 ml), N-methylpiperazine (29 ml), potassium carbonate (83 g) and ethanol (200 ml)was stirred and heated to reflux for 20 hours. The mixture was cooled to ambient temperature and filtered. The filtrate was evaporated and the residue was triturated under diethyl ether. The resultant mixture was filtered and the filtrate was evaporated. The residue was purified by distillation at about 60-70° C. under about 0.2 mm Hg to give 1-(3-hydroxypropyl)-4-methylpiperazine (17 g); NMR Spectrum: (CDCl3) 1.72 (m, 2H), 2.3 (s, 3H), 2.2-2.8 (m, 8H), 2.6 (t, 2H), 3.8 (t, 2H), 5.3 (br s, 1H).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06849625B2uspto-grants-2005_02