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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
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4-Oxatricyclo[5.2.2.0,2,6]undecane-3,5-dione → N-[4-{4-(2-pyrimidinyl)-1-piperazinyl}-butyl]bicyclo[2.2.2]octane-2,3-dicarboximide hydrochloride

HRID 1719868
ノート
印刷プレビュー

反応式

HRID 1719868 の反応式
[CH:1]12[CH2:8][CH2:7][CH:4]([CH2:5][CH2:6]1)[CH:3]1[C:9]([O:11][C:12](=[O:13])[CH:2]21)=O.[NH2:14][CH2:15][CH2:16][CH2:17][CH2:18][N:19]1[CH2:24][CH2:23][N:22]([C:25]2[N:30]=[CH:29][CH:28]=[CH:27][N:26]=2)[CH2:21][CH2:20]1.[ClH:31].C(O)(C)C>N1C=CC=CC=1>[ClH:31].[N:26]1[CH:27]=[CH:28][CH:29]=[N:30][C:25]=1[N:22]1[CH2:23][CH2:24][N:19]([CH2:18][CH2:17][CH2:16][CH2:15][N:14]2[C:12](=[O:13])[CH:2]3[CH:3]([CH:4]4[CH2:5][CH2:6][CH:1]3[CH2:8][CH2:7]4)[C:9]2=[O:11])[CH2:20][CH2:21]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 2522504-Oxatricyclo[5.2.2.0,2,6]undecane-3,5-dioneHCID 128407054-(2-Pyrimidinyl)-1-piperazinebutanamineHCID 21912024Isopropanol hydrochloride

生成物 1

HCID 13422629N-[4-{4-(2-pyrimidinyl)-1-piperazinyl}-butyl]bicyclo[2.2.2]octane-2,3-dicarboximide hydrochloride

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A mixture of bicyclo[2.2.2]octane-2,3-dicarboxylic anhydride (541 mg, 3 mmol), 1-(4-aminobutyl)-4-(2-pyrimidinyl)piperazine (708 mg, 3 mmol) and pyridine (12.1 ml) was refluxed for 10 hours. The solvent was removed from the mixture under reduced pressure. The residue was extracted with chloroform and water. The chloroform layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure to give crude crystals (1 g), which were treated with 6% hydrogen chloride/isopropanol. The solvent was removed to give N-[4-{4-(2-pyrimidinyl)-1-piperazinyl}-butyl]bicyclo[2.2.2]octane-2,3-dicarboximide hydrochloride (from ethanol). M.P. 198°-200° C.

後処理

  1. temperaturewas refluxed for 10 hours
  2. customThe solvent was removed from the mixture under reduced pressure
  3. extractionThe residue was extracted with chloroform and water
  4. dry with materialThe chloroform layer was dried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customto give crude crystals (1 g), which
  7. customThe solvent was removed

出典と根拠

ORDレコード
ord-f40515e51ca340ef9a33043b42030872
出典データセット
uspto-grants-1985_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04543355

反応ノート

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