Potassium Carbonate → 3-(4-Methyl-1-piperazine)propan-1-ol
반응식
Br[CH2:2][CH2:3][CH2:4][OH:5].[CH3:6][N:7]1[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]1.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[OH:5][CH2:4][CH2:3][CH2:2][N:10]1[CH2:11][CH2:12][N:7]([CH3:6])[CH2:8][CH2:9]1참가 물질
5
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).
후처리
- temperatureheated
- temperatureto reflux for 20 hours
- filtrationfiltered
- customThe filtrate was evaporated
- customthe residue was triturated under diethyl ether
- filtrationThe resultant mixture was filtered
- customthe filtrate was evaporated
- distillationThe residue was purified by distillation at about 60–70° C. under about 0.2 mm Hg
출처 및 근거
- ORD 기록
- ord-b7434b30502d4142a45c0be72fcadf4f
- 출처 데이터셋
- uspto-grants-2007_02
- 특허 번호
- US07173136B2
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