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Hydrochloric Acid → HCID 22903535、化合物

HRID 1440273
ノート
印刷プレビュー

反応式

HRID 1440273 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([C:12](=[O:37])[C:13]3[CH:18]=[CH:17][C:16]([NH:19][C:20](=[O:36])[C:21]4[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=4[O:27][CH2:28][CH2:29][CH2:30][C:31](OCC)=[O:32])=[N:15][CH:14]=3)[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[CH:38]=1.CO[BH-](OC)OC.[Na+].Cl>COCCOC>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([C:12](=[O:37])[C:13]3[CH:18]=[CH:17][C:16]([NH:19][C:20](=[O:36])[C:21]4[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=4[O:27][CH2:28][CH2:29][CH2:30][CH2:31][OH:32])=[N:15][CH:14]=3)[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[CH:38]=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 313Hydrochloric AcidHCID 3084262Sodium hydrotrimethoxyborate(1-)HCID 22903504HCID 22903504、化合物

生成物 1

HCID 22903535HCID 22903535、化合物収率 48.6%

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

実験手順

To a solution of 7-chloro-1-{6-[2-(3-ethoxycarbonylpropoxy)benzoyl-amino]nicotinoyl}-2,3,4,5-tetrahydro-1H-benzazepine (2.5 g)in ethylene glycol dimethyl ether (70 ml)is added sodium trimethoxyborohydride (3.78 g), and the mixture is refluxed for 3 hours. The reaction solution is gradually poured into diluted hydrochloric acid, and the mixture is extracted with ethyl acetate. The extract is washed with water, dried over magnesium sulfate, and evaporated under reduced pressure to remove the solvent. The residue is purified by silica gel column chromatography, and recrystallized from dichloromethane-diethyl ether to give 7-chloro-1-{6-[2-(4-hydroxybutoxy)benzoylamino]nicotinoyl}-2,3,4,5-tetrahydro-1H-benzazepine (1.12 g) as white powder.

後処理

  1. temperaturethe mixture is refluxed for 3 hours
  2. extractionthe mixture is extracted with ethyl acetate
  3. washThe extract is washed with water
  4. dry with materialdried over magnesium sulfate
  5. customevaporated under reduced pressure
  6. customto remove the solvent
  7. customThe residue is purified by silica gel column chromatography
  8. customrecrystallized from dichloromethane-diethyl ether

出典と根拠

ORDレコード
ord-b08d08924b71414d9c0b632494300ecc
出典データセット
uspto-grants-1996_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05498609

反応ノート

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