Hydrochloric Acid → 7-Methoxy-4-oxo-1,4-dihydroquinoline-6-carboxylic acid

HRID 387757ノート

反応式

HRID 387757 の反応式
OCC(CO)O.[OH-:7].[K+].[CH3:9][O:10][C:11]1[CH:20]=[C:19]2[C:14]([C:15](=[O:21])[CH:16]=[CH:17][NH:18]2)=[CH:13][C:12]=1[C:22]#N.Cl.[OH2:25]>>[CH3:9][O:10][C:11]1[CH:20]=[C:19]2[C:14]([C:15](=[O:21])[CH:16]=[CH:17][NH:18]2)=[CH:13][C:12]=1[C:22]([OH:25])=[O:7]

参加物

6

反応物 5

HCID 313Hydrochloric AcidHCID 753GlycerolHCID 962WaterHCID 14797Potassium HydroxideHCID 229363917-Methoxy-4-oxo-1,4-dihydroquinoline-6-carbonitrile

生成物 1

HCID 229364397-Methoxy-4-oxo-1,4-dihydroquinoline-6-carboxylic acid

反応条件

温度
160 °C

実験手順

Glycerol (20 ml) and potassium hydroxide (KOH, 3.0 g) were added to the 7-methoxy-4-oxo-1,4-dihydroquinoline-6-carbonitrile (2 g) of Production Example 24, and after heating and stirring at 160° C. for 3 hours, water (40 ml) was added and the mixture was heated at 80° C. for 30 minutes. After cooling, 2N hydrochloric acid was added to acidity and the precipitated insoluble portion was filtered out, washed with water and then dried under reduced pressure to obtain the title compound (1.6 g).

後処理

  1. temperatureafter heating
  2. temperaturethe mixture was heated at 80° C. for 30 minutes
  3. temperatureAfter cooling
  4. filtrationthe precipitated insoluble portion was filtered out
  5. washwashed with water
  6. customdried under reduced pressure

出典と根拠

ORDレコード
ord-778ff924cc67439b98cc979ce09b04b3
出典データセット
uspto-grants-2013_02
特許番号
US08372981B2

反応ノート

読み込み中…