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

HRID 489742

반응식

HRID 489742 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
60 °C

실험 절차

(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.

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 1.20 g (47.0%) of a white, crystalline powder, mp 148-150° C.

출처 및 근거

ORD 기록
ord-0bf00be2289647b3af150868dc494e11
출처 데이터셋
uspto-grants-2005_12
특허 번호
US06979695B2

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