Phosphorus oxychloride → 2-Chloro-6,7-dimethylquinoline-3-carbonitrile
反応式
[C:1]([C:3]1[C:4](=O)[NH:5][C:6]2[C:11]([CH:12]=1)=[CH:10][C:9]([CH3:13])=[C:8]([CH3:14])[CH:7]=2)#[N:2].P(Cl)(Cl)([Cl:18])=O>>[Cl:18][C:4]1[C:3]([C:1]#[N:2])=[CH:12][C:11]2[C:6](=[CH:7][C:8]([CH3:14])=[C:9]([CH3:13])[CH:10]=2)[N:5]=1参加物
3
実験手順
A mixture was prepared from 67.5 g of 3-cyano-6,7-dimethyl-2(1H)-quinolinone and 340 ml of phosphoryl chloride and this was heated at reflux for 18 hours. The mixture was cooled, excess phosphoryl chloride was removed by vacuum evaporation, and the residue was carefully added to water with vigorous stirring. The solid which formed was separated by filtration and recrystallized from methylene chloride to give 2-chloro-3-cyano-6,7-dimethylquinoline melting at about 189°-190° C.
後処理
- temperaturethis was heated
- temperatureat reflux for 18 hours
- temperatureThe mixture was cooled
- customexcess phosphoryl chloride was removed by vacuum evaporation
- additionthe residue was carefully added to water with vigorous stirring
- customThe solid which formed
- customwas separated by filtration
- customrecrystallized from methylene chloride
出典と根拠
- ORDレコード
- ord-0d595101550b4d03b90c8c286d071b75
- 出典データセット
- uspto-grants-1985_01
- 特許番号
- US04496569
反応ノート
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