Hydroxyamine hydrochloride → 2-Oxo-1,2-dihydroquinoline-3-carbonitrile

HRID 648444ノート

反応式

HRID 648444 の反応式
Cl.[NH2:2]O.[CH:4]([O-:6])=O.[Na+].ClC1[C:18]([CH:19]=O)=[CH:17][C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[N:10]=1>C(O)=O>[C:19]([C:18]1[C:4](=[O:6])[NH:10][C:11]2[C:16]([CH:17]=1)=[CH:15][CH:14]=[CH:13][CH:12]=2)#[N:2]

参加物

5

反応物 3

HCID 443297Hydroxyamine hydrochlorideHCID 6909582-Chloro-3-quinolinecarboxaldehydeHCID 2723810Sodium Formate

生成物 1

HCID 27645772-Oxo-1,2-dihydroquinoline-3-carbonitrile

試薬・触媒・溶媒 1

HCID 284Formic Acid溶媒

反応条件

温度
110 °C

実験手順

A mixture was prepared from 6 liters of 97% formic acid, 300 g of hydroxylamine hydrochloride, 500 g of sodium formate, and 700 g of 2-chloro-3-quinolinecarboxaldehyde and this mixture was heated to reflux (110° C.). The resulting solution was then maintained at 110° C. for 18 hours. The solution was then cooled and the solid which crystallized was separated by filtration and then successively washed twice with water, once with ethanol and once with methylene chloride to give 3-cyano-2(1H)-quinolinone.

後処理

  1. temperaturethis mixture was heated
  2. temperatureThe resulting solution was then maintained at 110° C. for 18 hours
  3. temperatureThe solution was then cooled
  4. customthe solid which crystallized
  5. customwas separated by filtration
  6. washsuccessively washed twice with water, once with ethanol and once with methylene chloride

出典と根拠

ORDレコード
ord-36a7a911eaf8413bb99086c7868056f7
出典データセット
uspto-grants-1988_04
特許番号
US04735948

反応ノート

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