反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[N:9]=[C:8]([C:13]#N)[CH:7]=[CH:6]2.[OH-:15].[Na+].C[OH:18]>>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[N:9]=[C:8]([C:13]([OH:18])=[O:15])[CH:7]=[CH:6]2参加物
4
反応条件
- 温度
- 120 °C
実験手順
6-Methoxy-quinoline-2-carbonitrile (9.3 g, 0.050 mol) in 96 ml methanol was treated with 240 ml of 20% NaOH and the mixture was heated to 120° C. in a sealed tube overnight. After cooling to 0° C. a precipitate appeared. The mixture was filtered to get a sodium salt that was suspended in water. HCl 25% was added until pH 3-4 to get the acid as a precipitate that was filtered and dried under vacuum. The mother liquid of the first filtration was acidified with HCl 25% until pH 3-4 until a precipitate appeared. The precipitate was filtered and the solid was washed in water and dried under vacuum to yield 9.6 g (86%) of the title compound as light brown solid. MS (m/e)=204 (M+H)+.
後処理
- temperatureAfter cooling to 0° C. a precipitate
- filtrationThe mixture was filtered
出典と根拠
- ORDレコード
- ord-684a65afc216472785d37d093bb33462
- 出典データセット
- uspto-grants-2009_05
- 特許番号
- US07534891B2
関連ノート
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