Potassium Carbonate → 3-(4-Methyl-1-piperazine)propan-1-ol
反応式
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]1参加物
5
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-b7434b30502d4142a45c0be72fcadf4f
- 出典データセット
- uspto-grants-2007_02
- 特許番号
- US07173136B2
反応ノート
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