反応 #2314283

ord-e3313ea46cd7402aa009ca69600977fe

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度cooled in an ice/ethanol bath
  2. 2
    workup.STIRRINGstirred for 30 minutes
  3. 3
    抽出The aqueous layer is extracted with dichloromethane
  4. 4
    洗浄the combined organic layers are sequentially washed with water, sodium bicarbonate, and water
  5. 5
    乾燥dried over magnesium sulfate
  6. 6
    濃縮The solution is concentrated in vacuo

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06413448B1uspto-grants-2002_07