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Ethyl chloroformate → 8-(2,6-Dichlorobenzoylamino)-4-(2-ethoxycarbonylhydrazino)quinoline

HRID 613550
ノート
印刷プレビュー

反応式

HRID 613550 の反応式
[Cl:1][C:2]1[CH:22]=[CH:21][CH:20]=[C:19]([Cl:23])[C:3]=1[C:4]([NH:6][C:7]1[CH:8]=[CH:9][CH:10]=[C:11]2[C:16]=1[N:15]=[CH:14][CH:13]=[C:12]2[NH:17][NH2:18])=[O:5].Cl[C:25]([O:27][CH2:28][CH3:29])=[O:26]>N1C=CC=CC=1.ClCCl>[Cl:1][C:2]1[CH:22]=[CH:21][CH:20]=[C:19]([Cl:23])[C:3]=1[C:4]([NH:6][C:7]1[CH:8]=[CH:9][CH:10]=[C:11]2[C:16]=1[N:15]=[CH:14][CH:13]=[C:12]2[NH:17][NH:18][C:25]([O:27][CH2:28][CH3:29])=[O:26])=[O:5]
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 2

HCID 10928Ethyl chloroformateHCID 19592850HCID 19592850、化合物

生成物 1

HCID 195928108-(2,6-Dichlorobenzoylamino)-4-(2-ethoxycarbonylhydrazino)quinoline収率 47.6%

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 6344Dichloromethane溶媒

実験手順

To a stirred suspension of 8-(2,6-dichlorobenzoylamino)-4-hydrazinoquinoline (200 mg) in pyridine (2 ml) was added a solution of ethyl chloroformate (68.8 mg) in dichloromethane (0.5 ml) under ice-cooling, and the mixture was stirred for 1 hour at ambient temperature. The mixture was concentrated in vacuo, and the residue was diluted with dichloromethane. The mixture was washed with water and brine, dried over magnesium sulfate and evaporated in vacuo. The residue was recrystallized from ethanol to give 8-(2,6-dichlorobenzoylamino)-4-(2-ethoxycarbonylhydrazino)quinoline (115 mg).

後処理

  1. temperaturecooling
  2. concentrationThe mixture was concentrated in vacuo
  3. additionthe residue was diluted with dichloromethane
  4. washThe mixture was washed with water and brine
  5. dry with materialdried over magnesium sulfate
  6. customevaporated in vacuo
  7. customThe residue was recrystallized from ethanol

出典と根拠

ORDレコード
ord-472603c746d749ac9556540b0217cb08
出典データセット
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06008230

反応ノート

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