反応式
[CH:1]([NH:4][C:5]1[CH:12]=[CH:11][CH:10]=[CH:9][C:6]=1[CH:7]=O)([CH3:3])[CH3:2].[C:13](OCC)(=[O:20])[CH2:14][C:15]([O:17][CH2:18][CH3:19])=[O:16].C(=O)([O-])O.[Na+]>C(OC(=O)C)(=O)C>[CH:1]([N:4]1[C:5]2[C:6](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH:7]=[C:14]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[C:13]1=[O:20])([CH3:3])[CH3:2]参加物
5
実験手順
A solution of 7.5 g of 2-isopropylaminobenzaldehyde, 11.0 g of diethyl malonate and 11.6 g of sodium hydrogen carbonate in 80 ml of acetic anhydride was stirred at 100° C. for 15 hours. After the solvent was removed by distillation in vacuo, water was added to the residue. The mixture was then extracted with ethyl acetate. After the organic layer was washed with water and then with saturated sodium bicarbonate aqueous solution, the organic layer was dried over anhydrous sodium sulfate. The solvent was distilled off in vacuum. The resulting oily substance was purified by silica gel column chromatography (n-hexane:ethyl acetate=4:1) to obtain 7.3 g of ethyl 1-isopropyl-2(1H)-quinolone-3-carboxylate.
後処理
- customAfter the solvent was removed by distillation in vacuo, water
- additionwas added to the residue
- extractionThe mixture was then extracted with ethyl acetate
- washAfter the organic layer was washed with water
- dry with materialwith saturated sodium bicarbonate aqueous solution, the organic layer was dried over anhydrous sodium sulfate
- distillationThe solvent was distilled off in vacuum
- customThe resulting oily substance was purified by silica gel column chromatography (n-hexane:ethyl acetate=4:1)
出典と根拠
- ORDレコード
- ord-6cbc130521414ee79d8e151e061a4437
- 出典データセット
- uspto-grants-1996_11
- 特許番号
- US05571820
関連ノート
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