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Ethoxyacetyl chloride → HCID 67051012、化合物

HRID 598314
ノート
印刷プレビュー

反応式

HRID 598314 の反応式
[CH2:1]([O:3][CH2:4][C:5](Cl)=O)[CH3:2].[CH2:8]([O:15][C:16]1[CH:17]=[C:18]2[C:23](=[CH:24][CH:25]=1)[N:22]=[CH:21][C:20]([NH2:26])=[C:19]2[NH:27][CH2:28][CH:29]([CH3:31])[CH3:30])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1>N1C=CC=CC=1>[CH2:8]([O:15][C:16]1[CH:25]=[CH:24][C:23]2[N:22]=[CH:21][C:20]3[N:26]=[C:5]([CH2:4][O:3][CH2:1][CH3:2])[N:27]([CH2:28][CH:29]([CH3:31])[CH3:30])[C:19]=3[C:18]=2[CH:17]=1)[C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 84189Ethoxyacetyl chlorideHCID 67050972HCID 67050972、化合物

生成物 1

HCID 67051012HCID 67051012、化合物収率 32.7%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

Ethoxyacetyl chloride (3.81 g, 31.1 mmol) was slowly added to a chilled solution of 6-benzyloxy-N4-(2-methylpropyl)quinoline-3,4-diamine (9.1 g, 28.3 mmol) in pyridine (60 mL). The reaction was allowed to warm to ambient temperature and then heated at reflux for three hours. The solvent was removed under reduced pressure, and the residue was dissolved in dichloromethane (200 mL). The resulting solution was washed with water (3×100 mL) and concentrated under reduced pressure. The concentrated solution was passed through a layer of silica gel (eluting with dichloromethane:methanol 95:5) and concentrated under reduced pressure to provide 3.6 g of 8-benzyloxy-2-ethoxymethyl-1-(2-methylpropyl)-1H-imidazo[4,5-c]quinoline as an oil.

後処理

  1. temperatureheated
  2. temperatureat reflux for three hours
  3. customThe solvent was removed under reduced pressure
  4. dissolutionthe residue was dissolved in dichloromethane (200 mL)
  5. washThe resulting solution was washed with water (3×100 mL)
  6. concentrationconcentrated under reduced pressure
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-35d874c59e8d492aaeea46ba244f0fce
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07897597B2

反応ノート

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