Hydrochloric Acid → 4-Methoxyphenyl (4-(4-methyl-3-pentenyl)-3-cyclohexenyl)methyl ketone
反応式
[CH3:1][C:2]([CH3:16])=[CH:3][CH2:4][CH2:5][C:6]1[CH2:11][CH2:10][CH:9]([CH2:12][C:13](Cl)=[O:14])[CH2:8][CH:7]=1.[C:17]1([O:23][CH3:24])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.Cl>ClCCl>[CH3:1][C:2]([CH3:16])=[CH:3][CH2:4][CH2:5][C:6]1[CH2:11][CH2:10][CH:9]([CH2:12][C:13]([C:20]2[CH:21]=[CH:22][C:17]([O:23][CH3:24])=[CH:18][CH:19]=2)=[O:14])[CH2:8][CH:7]=1参加物
5
実験手順
A solution of acid chloride 2C (R=4-Methyl-3-pentenyl) (10 g) in anhydrous dichloromethane (100 mL) is added dropwise to a mixture of ferric chloride (7.8 g) and anisole 2D (4.5 g) in dichloromethane (175 mL), cooled in an ice/ethanol bath. The resulting mixture is gradually warmed to room temperature and stirred overnight. The mixture is poured into 25% HCl (150 mL) and stirred for 30 minutes. The aqueous layer is extracted with dichloromethane, and the combined organic layers are sequentially washed with water, sodium bicarbonate, and water, then dried over magnesium sulfate. The solution is concentrated in vacuo.
後処理
- temperaturecooled in an ice/ethanol bath
- stirringstirred for 30 minutes
- extractionThe aqueous layer is extracted with dichloromethane
- washthe combined organic layers are sequentially washed with water, sodium bicarbonate, and water
- dry with materialdried over magnesium sulfate
- concentrationThe solution is concentrated in vacuo
出典と根拠
- ORDレコード
- ord-e3313ea46cd7402aa009ca69600977fe
- 出典データセット
- uspto-grants-2002_07
- 特許番号
- US06413448B1
反応ノート
読み込み中…