Potassium Carbonate → 3-(4-Methyl-1-piperazine)propan-1-ol

HRID 347323

反応式

HRID 347323 の反応式
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

反応物 3

HCID 11430Potassium CarbonateHCID 123083-Bromo-1-propanolHCID 531671-Methylpiperazine

生成物 1

HCID 792083-(4-Methyl-1-piperazine)propan-1-ol

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

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

  1. temperatureheated
  2. temperatureto reflux for 20 hours
  3. filtrationfiltered
  4. customThe filtrate was evaporated
  5. customthe residue was triturated under diethyl ether
  6. filtrationThe resultant mixture was filtered
  7. customthe filtrate was evaporated
  8. 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

関連ノート

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