反応式
[Cl-].[Cl-].[Cl-].[Al+3].[C:5](Cl)(=[O:7])[CH3:6].[Cl:9][CH2:10][CH2:11][CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.Cl>C(Cl)Cl>[Cl:9][CH2:10][CH2:11][CH2:12][C:13]1[CH:18]=[CH:17][C:16]([C:5](=[O:7])[CH3:6])=[CH:15][CH:14]=1参加物
6
反応条件
- 温度
- -7 °C
実験手順
84 mL of CH2Cl2 and 14.4 g (1.1 eq.) of aluminum trichloride (AlCl3) are placed in a reactor at 20° C. with stirring. The reaction medium is cooled to −7° C. and 8.5 g (1.1 eq.) of acetyl chloride are then added. The mixture is stirred for 30 minutes and 15 g of 1-chloro-3-phenylpropane are then added at 0° C. At the end of the reaction, the reaction mixture is poured over about 30 minutes with vigorous stirring into 75 mL of 5% hydrochloric acid solution. The mixture is stirred for 1 hour at 10° C., the phases are then separated by settling and the aqueous phase is extracted with CH2Cl2. The organic phases are combined and washed successively with 2N HCl solution, 1N sodium hydroxide solution and water.
後処理
- stirringThe mixture is stirred for 30 minutes
- customAt the end of the reaction
- additionthe reaction mixture is poured over about 30 minutes
- stirringThe mixture is stirred for 1 hour at 10° C.
- customthe phases are then separated
- extractionthe aqueous phase is extracted with CH2Cl2
- washwashed successively with 2N HCl solution, 1N sodium hydroxide solution and water
出典と根拠
- ORDレコード
- ord-e1c4a911af3341c69a25d1c924234ada
- 出典データセット
- uspto-grants-2014_06
- 特許番号
- US08748636B2
関連ノート
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