反応式
[OH-:1].[K+].[CH3:3][S:4][C:5]1[CH:6]=[C:7]2[C:11](=[CH:12][CH:13]=1)[NH:10][C:9](=[O:14])[C:8]2=O.[F:16][C:17]([F:29])([F:28])[C:18]1[CH:19]=[C:20]([C:24](=O)[CH2:25][CH3:26])[CH:21]=[CH:22][CH:23]=1>O.C(O)C>[CH3:26][C:25]1[C:24]([C:20]2[CH:21]=[CH:22][CH:23]=[C:18]([C:17]([F:16])([F:28])[F:29])[CH:19]=2)=[N:10][C:11]2[C:7]([C:8]=1[C:9]([OH:14])=[O:1])=[CH:6][C:5]([S:4][CH3:3])=[CH:13][CH:12]=2参加物
6
実験手順
Potassium hydroxide (3.31 g, 59.0 mmol) in water (10 mL) was added slowly to a suspension of 5-(methylthio)-1H-indole-2,3-dione (1.9 g, 9.83 mmol) in ethanol (25 mL). 1-[3-(Trifluoromethyl)phenyl]-1-propanone (1.99 g, 9.83 mmol) was added and the mixture was heated to reflux for 1 h. The solvent was removed under reduced pressure, the residue was dissolved in water, and the aqueous mixture was washed with ether (3 times). The aqueous phase was chilled and was acidified to pH 3 with concentrated HCl. The solid material was collected by filtration, washed with water, and air dried to afford 3-methyl-6-(methylthio)-2-[3-(trifluoromethyl)phenyl]-4-quinolinecarboxylic acid (2.5 g, 67% yield). MS (m/z) 378.0 (M+H+).
後処理
- temperaturethe mixture was heated
- temperatureto reflux for 1 h
- customThe solvent was removed under reduced pressure
- dissolutionthe residue was dissolved in water
- washthe aqueous mixture was washed with ether (3 times)
- temperatureThe aqueous phase was chilled
- filtrationThe solid material was collected by filtration
- washwashed with water, and air
- customdried
出典と根拠
- ORDレコード
- ord-20820fad8d1647319b9ca15de2fd2c09
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08658636B2
関連ノート
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