反応式
[CH:1]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)([CH2:3][CH3:4])[CH3:2].P(Cl)(Cl)(Cl)(Cl)Cl.[Cl:17][S:18](O)(=[O:20])=[O:19]>ClCCCl>[CH:1]([C:5]1[CH:10]=[CH:9][C:8]([S:18]([Cl:17])(=[O:20])=[O:19])=[CH:7][CH:6]=1)([CH2:3][CH3:4])[CH3:2]参加物
5
反応条件
- 温度
- 80 °C
実験手順
To a solution of commercially available sec-butylbenzene (1.34 g; 10 mmol) in 1,2-dichloroethane (50 mL) was added phosphorus pentachloride (2.5 g; 12 mmol) followed by chlorosulfonic acid (1.3 mL; 20 mmol) slowly. The mixture was heated at 80° C. overnight, then cooled to room temperature and mixed with ice water (150 mL). The organic phase was separated, and the aqueous phase was extracted with dichloromethane (2×10 mL). The organic phases were combined and dried over magnesium sulfate and concentrated under reduced pressure to give an orange oil which was used without further purification (2.3 g).
後処理
- temperaturecooled to room temperature
- customThe organic phase was separated
- extractionthe aqueous phase was extracted with dichloromethane (2×10 mL)
- dry with materialdried over magnesium sulfate
- concentrationconcentrated under reduced pressure
- customto give an orange oil which
- customwas used without further purification (2.3 g)
出典と根拠
- ORDレコード
- ord-b8e394d90157493fba6a2bb1d270ca01
- 出典データセット
- uspto-grants-2012_05
- 特許番号
- US08178699B2
関連ノート
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