2,3-Dihydroxybutanedioic Acid → 3-[4-(2-Pyridyl)piperidin-1-yl]propylamine l-tartrate salt

HRID 429953ノート

反応式

HRID 429953 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH:7]1[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][CH2:15][NH2:16])[CH2:9][CH2:8]1.[C:17]([OH:26])(=[O:25])[C@@H:18]([C@H:20]([C:22]([OH:24])=[O:23])[OH:21])[OH:19].C(O)(=O)C(C(C(O)=O)O)O>C(O)C>[C:22]([C@@H:20]([C@H:18]([C:17]([OH:26])=[O:25])[OH:19])[OH:21])([OH:24])=[O:23].[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH:7]1[CH2:8][CH2:9][N:10]([CH2:13][CH2:14][CH2:15][NH2:16])[CH2:11][CH2:12]1

参加物

5

反応物 3

HCID 8752,3-Dihydroxybutanedioic Acid2 回HCID 444305L-Tartaric acidHCID 101768154-(2-pyridinyl)-1-Piperidinepropanamine

生成物 1

HCID 701512003-[4-(2-Pyridyl)piperidin-1-yl]propylamine l-tartrate salt

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

A solution of 3-[4-(2-pyridyl)piperidin-1-yl]propylamine, (6), (637.9 g, 3.86 mol) in ethanol (8.5 L) was warmed to 65° C. A solution of L-tartaric acid (637.9 g, 4.25 mol) in ethanol (2.23 L) was added in portions. Approximately 15% of the tartaric acid solution was added and then reaction mixture was aged for 1 hour to afford a thin slurry of crystalline material. The remaining tartaric acid solution was added dropwise. Heating was discontinued and the solution was slowly cooled to ambient temperature overnight. The solids were filtered, rinsed with ethanol (2×1 L) and dried under a stream of nitrogen to afford 3-[4-(2-pyridyl)piperidin-1-yl]propylamine L-tartrate salt, (7), as a pale yellow solid.

後処理

  1. customreaction mixture
  2. customto afford a thin slurry of crystalline material
  3. temperatureHeating
  4. filtrationThe solids were filtered
  5. washrinsed with ethanol (2×1 L)
  6. customdried under a stream of nitrogen

出典と根拠

ORDレコード
ord-b42109ac54cf43b2b9777bd9c1d495e6
出典データセット
uspto-grants-2001_11
特許番号
US06320049B1

反応ノート

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