Water → (4E)-N-Methyl-5-(3-pyridyl)-4-penten-2-amine Hemigalactarate

HRID 489742

反応式

HRID 489742 の反応式
[CH3:1][NH:2][CH:3]([CH2:5]/[CH:6]=[CH:7]/[C:8]1[CH:9]=[N:10][CH:11]=[CH:12][CH:13]=1)[CH3:4].[O:14]=[C:15]([OH:27])[C@@H:16]([C@H:18]([C@H:20]([C@@H:22]([C:24]([OH:26])=[O:25])[OH:23])[OH:21])[OH:19])[OH:17].O>C(O)C>[O:14]=[C:15]([OH:27])[C@@H:16]([C@H:18]([C@H:20]([C@@H:22]([C:24]([OH:26])=[O:25])[OH:23])[OH:21])[OH:19])[OH:17].[CH3:1][NH:2][CH:3]([CH2:5]/[CH:6]=[CH:7]/[C:8]1[CH:9]=[N:10][CH:11]=[CH:12][CH:13]=1)[CH3:4].[CH3:1][NH:2][CH:3]([CH2:5]/[CH:6]=[CH:7]/[C:8]1[CH:9]=[N:10][CH:11]=[CH:12][CH:13]=1)[CH3:4]

参加物

5

反応物 3

HCID 962WaterHCID 3037582Galactaric acidHCID 10219654(4E)-N-Methyl-5-(3-pyridyl)-4-penten-2-amine

生成物 1

HCID 131722555(4E)-N-Methyl-5-(3-pyridyl)-4-penten-2-amine Hemigalactarate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
60 °C

実験手順

(4E)-N-Methyl-5-(3-pyridyl)-4-penten-2-amine (1.60 g, 9.10 mmol) was dissolved in ethyl alcohol (20 mL), assisted by warming to 60° C. The warm solution was treated with galactaric acid (955 mg, 4.54 mmol) in one portion, followed by the dropwise addition of water (0.5 mL). The solution was filtered while hot to remove some insoluble material. The filtrate was allowed to cool to ambient temperature. The resulting crystals were filtered, washed with anhydrous diethyl ether, and dried under vacuum at 40° C. to yield 1.20 g (47.0%) of a white, crystalline powder, mp 148-150° C.

後処理

  1. filtrationThe solution was filtered while hot
  2. customto remove some insoluble material
  3. temperatureto cool to ambient temperature
  4. filtrationThe resulting crystals were filtered
  5. washwashed with anhydrous diethyl ether
  6. customdried under vacuum at 40° C.
  7. customto yield 1.20 g (47.0%) of a white, crystalline powder, mp 148-150° C.

出典と根拠

ORDレコード
ord-0bf00be2289647b3af150868dc494e11
出典データセット
uspto-grants-2005_12
特許番号
US06979695B2

関連ノート

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