反応式
C(N(CC)[CH2:4][CH2:5][C:6](=[O:19])[CH2:7][CH:8]([CH3:18])[CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([O:16][CH3:17])[CH:11]=1)C.CC(CC1C=CC=C(OC)C=1)CC(=O)C=C.[CH2:38]([CH:40]1[C:44](=[O:45])[CH2:43][CH2:42][C:41]1=[O:46])[CH3:39]>[OH-].[K+]>[CH2:38]([C:40]1([CH2:4][CH2:5][C:6](=[O:19])[CH2:7][CH:8]([CH3:18])[CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([O:16][CH3:17])[CH:11]=2)[C:44](=[O:45])[CH2:43][CH2:42][C:41]1=[O:46])[CH3:39]参加物
5
実験手順
Add a mixture of 1-diethylamino-6-(m-methoxyphenyl)-5-methylhexan-3-one and 5-methyl-6-(m-methoxyphenyl)hex-1-en-3-one (6 g, prepared by slow distillation of the former substance) to 2-ethylcyclopentane-1,3-dione (3.5 g) in 0.12% methanolic potassium hydroxide (10 cc) and heat the mixture under reflux for 6 hours. Remove most of the solvent under reduced pressure and add ether (25 cc) and benzene (25 cc) to the residue. Wash the solution with 5% aqueous sodium hydroxide, water, dilute hydrochloric acid, and brine, and dry. Evaporate the solvent to obtain a viscous brown gum, which is the triketone 2-ethyl-2-(6-m-methoxyphenyl-5-methyl-3-oxohexyl)cyclopentane-1,3-dione.
後処理
- additionAdd
- temperatureheat the mixture
- temperatureunder reflux for 6 hours
- customRemove most of the solvent under reduced pressure
- additionadd ether (25 cc) and benzene (25 cc) to the residue
- washWash the solution with 5% aqueous sodium hydroxide, water, dilute hydrochloric acid, and brine
- customdry
- customEvaporate the solvent
- customto obtain a viscous brown gum, which
出典と根拠
- ORDレコード
- ord-7a35113cc7024972af5d9d45f8589e0a
- 出典データセット
- uspto-grants-1976_05
- 特許番号
- US03959322
関連ノート
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