反応式
[F:1][C:2]([F:15])([F:14])[C:3]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[CH:8]=[CH:7][C:4]=1[CH:5]=O.[CH3:16][C:17](=[O:22])[CH2:18][C:19](=[O:21])[CH3:20].C(O)(=O)C.N1CCCCC1>ClCCl>[N+:11]([C:9]1[CH:8]=[CH:7][C:4]([CH:5]=[C:18]([C:17](=[O:22])[CH3:16])[C:19](=[O:21])[CH3:20])=[C:3]([C:2]([F:15])([F:14])[F:1])[CH:10]=1)([O-:13])=[O:12]参加物
6
実験手順
1 g (4.56 mmol) of 2-trifluoromethyl-4-nitrobenzaldehyde, 0.51 ml (5.02 mmol) of 2,4-pentanedione, 0.4 ml (6.85 mmol) of acetic acid and 90 μl (0.91 mmol) of piperidine in 20 ml of anhydrous dichloromethane are stirred under reflux with a water trap for 24 h. After cooling, the reaction solution is washed successively with saturated sodium bicarbonate solution and saturated sodium chloride solution. The organic phase is dried over magnesium sulfate and concentrated. The residue (1.28 g) is reacted in the next stage without further purification.
後処理
- temperatureunder reflux with a water trap for 24 h
- temperatureAfter cooling
- washthe reaction solution is washed successively with saturated sodium bicarbonate solution and saturated sodium chloride solution
- dry with materialThe organic phase is dried over magnesium sulfate
- concentrationconcentrated
- customThe residue (1.28 g) is reacted in the next stage without further purification
出典と根拠
- ORDレコード
- ord-83ac0246cdb4453b984f57c40650b2e2
- 出典データセット
- uspto-grants-2013_03
- 特許番号
- US08404709B2
関連ノート
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