反応 #9723

ord-ac4f6997785540cfabd1e40607d0df66

反応条件

温度
40°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The organic layer was collected
  2. 2
    洗浄washed twice with water and brine
  3. 3
    乾燥dried over sodium sulfate
  4. 4
    ろ過filtered
  5. 5
    濃縮the filtrate concentrated

実験手順

A solution of ethyl 2-(4-acetyl-2-methylphenoxy)-2-methylpropanoate (intermediate 8, 37.33 g) in dichloromethane (650 ml) was treated with 4-toluenesulphonic acid (2.75 g) followed by m-chloroperbenzoic acid (60.5 g) and the mixture warmed to 40° C. and stirred under nitrogen for 19 hours. The cooled mixture was treated with dichloromethane (350 ml) and the resulting mixture added to aqueous potassium iodide (1000 ml, 10% solution). The organic layer was collected and washed twice with water and brine, then dried over sodium sulfate, filtered and the filtrate concentrated to give the title compound as an orange oil.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07091237B2uspto-grants-2006_08