反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:9][CH2:10][C:11]([CH3:13])=[CH2:12])=[C:4]([CH:14]([CH3:16])[CH3:15])[CH:3]=1.[Cl-].[Al+3].[Cl-].[Cl-].[OH-].[Na+]>ClCCl>[Br:1][C:2]1[CH:7]=[C:6]2[C:5](=[C:4]([CH:14]([CH3:16])[CH3:15])[CH:3]=1)[O:8][CH2:9][CH2:10][C:11]2([CH3:13])[CH3:12]参加物
5
反応条件
- 温度
- 0 °C
実験手順
4-Bromo-1-[(3-methylbut-3-en-1-yl)oxy]-2-(propan-2-yl)benzene (293 mg, 1.03 mmol) dissolved in dichloromethane (3.10 mL) was cooled to 0° C. and aluminum chloride (138 mg, 1.03 mmol) in dichloromethane (3.0 mL) was added via a syringe. The reaction mixture was stirred at 0° C. for 30 minutes. It was then poured into an Erlenmeyer flask containing a 10% aqueous NaOH solution and ice. The mixture was extracted with dichloromethane (2×), and the combined organic layers were dried over Na2SO4, filtered, and concentrated under vacuum. The crude residue was purified by silica gel chromatography, eluting with 0-10% EtOAc/Hexanes to give the title compound as a colorless oil.
後処理
- additionIt was then poured into an Erlenmeyer flask
- extractionThe mixture was extracted with dichloromethane (2×)
- dry with materialthe combined organic layers were dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated under vacuum
- customThe crude residue was purified by silica gel chromatography
- washeluting with 0-10% EtOAc/Hexanes
出典と根拠
- ORDレコード
- ord-6e14fb9c9c2147cc8acc6489354063c2
- 出典データセット
- uspto-grants-2014_06
- 特許番号
- US08742110B2
関連ノート
読み込み中…