반응 #51047
ord-8cae2a34954640a9b6a0abd424a54f32
용매
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도heated
- 2온도to reflux for 20 hours
- 3여과filtered
- 4기타The filtrate was evaporated
- 5기타the residue was triturated under diethyl ether
- 6여과The resultant mixture was filtered
- 7기타the filtrate was evaporated
- 8workup.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).