Hydrochloric Acid → 3-Quinolinecarbonitrile, 4-hydroxy-
反応式
CN([CH:4]=[N:5][C:6]1[CH:15]=[CH:14][CH:13]=[CH:12][C:7]=1[C:8]([O:10]C)=O)C.C[O-].[Na+].[C:19](#[N:21])[CH3:20].Cl>O.C1(C)C=CC=CC=1>[O:10]=[C:8]1[C:7]2[C:6](=[CH:15][CH:14]=[CH:13][CH:12]=2)[NH:5][CH:4]=[C:20]1[C:19]#[N:21]参加物
7
実験手順
A stirred mixture of 1.03 g of methyl 2-(dimethylaminomethyleneamino)benzoate, 0.54 g of sodium methoxide, 1.04 ml of acetonitrile, and 10 ml of toluene was refluxed for 18 h. The mixture was cooled, treated with water, and brought to pH 3 by addition of dilute HCl. The resulting solid was extracted with ethyl acetate. The extract was washed with water, dried and evaporated. The residue was recrystallized from ethanol to give a solid, mp 290-300° C.
後処理
- temperaturewas refluxed for 18 h
- temperatureThe mixture was cooled
- extractionThe resulting solid was extracted with ethyl acetate
- washThe extract was washed with water
- customdried
- customevaporated
- customThe residue was recrystallized from ethanol
- customto give a solid, mp 290-300° C.
出典と根拠
- ORDレコード
- ord-f9e34bda3027493b83d4e328ef761266
- 出典データセット
- uspto-grants-2002_05
- 特許番号
- US06384051B1
反応ノート
読み込み中…