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Dimethylformamide → Quinoline-6-carbonyl chloride

HRID 70810
ノート
印刷プレビュー

反応式

HRID 70810 の反応式
[N:1]1[C:10]2[C:5](=[CH:6][C:7]([C:11]([OH:13])=O)=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.CN(C)C=O.C(Cl)(=O)C([Cl:22])=O>ClCCl>[N:1]1[C:10]2[C:5](=[CH:6][C:7]([C:11]([Cl:22])=[O:13])=[CH:8][CH:9]=2)[CH:4]=[CH:3][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 6228DimethylformamideHCID 65578Oxalyl chlorideHCID 825716-Quinolinecarboxylic acid

生成物 1

HCID 12391963Quinoline-6-carbonyl chloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Quinoline-6-carboxylic acid (1.4 g) was dissolved in dichloromethane (50 ml). N,N-dimethylformamide (100 μL) and oxalyl chloride (1.6 g) were added to this solution at room temperature and stirred for two hours followed by reflux for 20 minutes. The solvent was removed by distillation under the reduced pressure to obtain crude quinoline-6-carbonyl chloride. It was dissolved in pyridine and added to 2-bromo-4-(1-bromo-1,1,2,3,3,3-hexafluoropropan-2-yl)-6-(difluoromethoxy)aniline (0.73 g) also dissolved in pyridine, and the resulting mixture was heated under reflux for 5 hours. After cooling to room temperature, the reaction solution was diluted with 1 N hydrochloric acid and extracted twice with ethyl acetate. The solvent was removed by distillation under the reduced pressure. The resulting residues were dissolved in tetrahydrofiaran (30 ml), added with 1 M aqueous solution of lithium hydroxide (50 ml), and stirred at room temperature for 2 hours. The reaction solution was extracted twice with ethyl acetate. The organic phases were combined, washed with water, and dried over anhydrous magnesium sulfate. The drying agent (anhydrous magnesium sulfate) was removed by filtration and the solvent was distilled off under the reduced pressure. The resulting residues were purified by column chromatography to obtain N-[2-bromo-4-(1-bromo-1,1,2,3,3,3-hexafluoropropan-2-yl)-6-(difluoromethoxy)phenyl]quinoline-6-carboxamide (0.84 g, 86%).

後処理

  1. temperatureby reflux for 20 minutes
  2. customThe solvent was removed by distillation under the reduced pressure

出典と根拠

ORDレコード
ord-9ca84f55af33497c8d7af281800f7c96
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08822691B2

反応ノート

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