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

HRID 489750노트

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HRID 489750 반응식
[CH3:1][NH:2][C@H: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][C@H: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][C@H:3]([CH2:5]/[CH:6]=[CH:7]/[C:8]1[CH:9]=[N:10][CH:11]=[CH:12][CH:13]=1)[CH3:4]

참가 물질

5

반응물 3

HCID 962WaterHCID 3037582Galactaric acidHCID 98341074-Penten-2-amine, N-methyl-5-(3-pyridinyl)-, (2S,4E)-

생성물 1

HCID 131722557(2S)-(4E)-N-Methyl-5-(3-pyridyl)-4-penten-2-amine Hemigalactarate

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
60 °C

실험 절차

(2S)-(4E)-N-Methyl-5-(3-pyridyl)-4-penten-2-amine (800 mg, 4.54 mmol) was dissolved in ethyl alcohol (20 mL), assisted by warming to 60° C. The warm solution was treated with galactaric acid (477 mg, 2.27 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 830 mg (65.4%) of an off-white, crystalline powder, mp 141-143° C.

후처리

  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 830 mg (65.4%) of an off-white, crystalline powder, mp 141-143° C.

출처 및 근거

ORD 기록
ord-313a78203ec348d5bc8d3f31b9ec70c9
출처 데이터셋
uspto-grants-2005_12
특허 번호
US06979695B2

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