反応式
[Na].[CH2:2]([N:6]([CH2:17][CH2:18][CH2:19][CH3:20])[C:7]1[CH:14]=[CH:13][C:10]([CH:11]=O)=[C:9]([O:15][CH3:16])[CH:8]=1)[CH2:3][CH2:4][CH3:5].[CH2:21]([C:25]1[C:26](=[O:34])[CH2:27][C:28]([CH3:33])([CH3:32])[CH2:29][C:30]=1[CH3:31])[CH2:22][CH2:23][CH3:24].C([O-])(=O)C.[NH4+]>C(O)C.C(OCC)(=O)C>[CH2:2]([N:6]([CH2:17][CH2:18][CH2:19][CH3:20])[C:7]1[CH:14]=[CH:13][C:10]([CH:11]=[CH:31][C:30]2[CH2:29][C:28]([CH3:32])([CH3:33])[CH2:27][C:26](=[O:34])[C:25]=2[CH2:21][CH2:22][CH2:23][CH3:24])=[C:9]([O:15][CH3:16])[CH:8]=1)[CH2:3][CH2:4][CH3:5]参加物
7
反応物 4
生成物 1
試薬・触媒・溶媒 2
反応条件
- 温度
- 60 °C
実験手順
0.3 g (13.0 mmol) of sodium was dissolved in 15 ml of ethanol. Next, 2.63 g (10.0 mmol) of 4-dibutylamino-2-methoxybenzaldehyde and 2.22 g (11.0 mmol) of 2-butyl-3,5,5-trimethyl-2-cyclohexenone were dissolved in 5 ml of ethanol and added to the mixture. To this mixture, 0.36 g of ammonium acetate was added and the mixture was stirred with heating at 60° C. for 22 hours. To the mixture, 100 ml of ethyl acetate was added. Washing with a saturated saline solution, drying over anhydrous sodium sulfate, and concentration were performed. The residual liquid was purified by silica gel column chromatography to give 465 mg of a dark red oily matter (yield: 10.6%).
後処理
- additionadded to the mixture
- washWashing with a saturated saline solution
- dry with materialdrying over anhydrous sodium sulfate, and concentration
- customThe residual liquid was purified by silica gel column chromatography
- customto give 465 mg of a dark red oily matter (yield: 10.6%)
出典と根拠
- ORDレコード
- ord-3c4daaf907ac4998a292cf2de3c55ec4
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08846955B2
関連ノート
読み込み中…