ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Water → 4-(3-Pyridyloxy)butylamine Hemigalactarate

HRID 1168922
ノート
印刷プレビュー

反応式

HRID 1168922 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([O:7][CH2:8][CH2:9][CH2:10][CH2:11][NH2:12])[CH:2]=1.[O:13]=[C:14]([OH:26])[C@@H:15]([C@H:17]([C@H:19]([C@@H:21]([C:23]([OH:25])=[O:24])[OH:22])[OH:20])[OH:18])[OH:16].O>C(O)C>[O:13]=[C:14]([OH:26])[C@@H:15]([C@H:17]([C@H:19]([C@@H:21]([C:23]([OH:25])=[O:24])[OH:22])[OH:20])[OH:18])[OH:16].[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([O:7][CH2:8][CH2:9][CH2:10][CH2:11][NH2:12])[CH:2]=1.[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([O:7][CH2:8][CH2:9][CH2:10][CH2:11][NH2:12])[CH:2]=1
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 121122194-(Pyridin-3-yloxy)butan-1-amine

生成物 1

HCID 121122184-(3-Pyridyloxy)butylamine Hemigalactarate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 4-(3-pyridyloxy)butylamine (1.25 g, 7.50 mmol) in ethanol (12 mL) was added galactaric acid (0.791 g, 3.76 mmol). Water (3 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) (4 mL). The filtrate was diluted with ethanol (30 mL). The mixture was allowed to cool to ambient temperature and was further cooled at 5° C. for 48 h. Very few solids precipitated. Consequently, the solution was concentrated to a flaky solid. The product was slurried in 2-propanol, and the 2-propanol was decanted. The product was vacuum dried at 40° C. to give 1.28 g (62.7%) of fine, white powder, mp 177-180° C. The compound exhibits a Ki of 232 nM; the effect at muscle sites is 0 percent; and the effect at ganglia sites is 11 percent. The compound exhibits neurotransmitter release of 100 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 (30 mL)
  7. temperaturewas further cooled at 5° C. for 48 h
  8. customVery few solids precipitated
  9. concentrationConsequently, the solution was concentrated to a flaky solid
  10. customthe 2-propanol was decanted
  11. customdried at 40° C.
  12. customto give 1.28 g (62.7%) of fine, white powder, mp 177-180° C

出典と根拠

ORDレコード
ord-09684964dc364937911aa3687b994d96
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

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート