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Water → Ethyl(3-(3-pyridyloxy)propyl)amine Hemigalactarate

HRID 1168959
ノート
印刷プレビュー

反応式

HRID 1168959 の反応式
[CH2:1]([NH:3][CH2:4][CH2:5][CH2:6][O:7][C:8]1[CH:9]=[N:10][CH:11]=[CH:12][CH:13]=1)[CH3:2].[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].[CH2:1]([NH:3][CH2:4][CH2:5][CH2:6][O:7][C:8]1[CH:9]=[N:10][CH:11]=[CH:12][CH:13]=1)[CH3:2].[CH2:1]([NH:3][CH2:4][CH2:5][CH2:6][O:7][C:8]1[CH:9]=[N:10][CH:11]=[CH:12][CH:13]=1)[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 3037582Galactaric acidHCID 9877539Ethyl(3-(3-pyridyloxy)propyl)amine

生成物 1

HCID 12112226Ethyl(3-(3-pyridyloxy)propyl)amine Hemigalactarate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of ethyl(3-(3-pyridyloxy)propyl)amine (400 mg, 2.20 mmol) in ethanol (11 mL) was added galactaric acid (233 mg, 1.10 mmol). Water (3.5 mL) was added drop-wise, while warming the solution to reflux. To remove some white, insoluble solids, the warm solution was filtered through a glass wool plug, washing the filter plug with a warm solution of ethanol-water (4:1, v/v) (3.5 mL). The filtrate was diluted with ethanol (17 mL). The mixture was allowed to cool to ambient temperature and was further cooled at 5° C. Very few solids precipitated. Consequently, the solution was concentrated to a residue that was vacuum dried. The solids were slurried in 2-propanol, and the 2-propanol was evaporated. The resulting solids were slurried in anhydrous ether. The product was filtered, washed with ether, and vacuum dried at 40° C. to give 348 mg (55.0%) of a brown, flaky powder, mp 147-150° C. The compound exhibits a Ki of 66 nM; the effect at muscle sites is 13 percent; and the effect at ganglia sites is 13 percent. The compound exhibits neurotransmitter release of 57 percent.

後処理

  1. temperaturewhile warming the solution
  2. temperatureto reflux
  3. customTo remove some white, insoluble solids
  4. filtrationthe warm solution was filtered through a glass wool plug
  5. washwashing the filter plug with a warm solution of ethanol-water (4:1
  6. additionThe filtrate was diluted with ethanol (17 mL)
  7. temperaturewas further cooled at 5° C
  8. customVery few solids precipitated
  9. concentrationConsequently, the solution was concentrated to a residue that
  10. customdried
  11. customthe 2-propanol was evaporated
  12. filtrationThe product was filtered
  13. washwashed with ether, and vacuum
  14. customdried at 40° C.
  15. customto give 348 mg (55.0%) of a brown, flaky powder, mp 147-150° C

出典と根拠

ORDレコード
ord-5894e74266f945f992a1ff6ada0b8d3b
出典データセット
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06627648B1

反応ノート

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