反応 #346839

ord-4cec5fb0ee97485c9bd8bce822d61aa2

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度reflux temperature for approximately 24 hours
  2. 2
    温度The reaction mixture is cooled
  3. 3
    抽出extracted with methylene chloride
  4. 4
    洗浄The extract is washed with water
  5. 5
    乾燥a solution of 2 N sodium hydroxide, dried over anhydrous sodium sulfate
  6. 6
    その他evaporated in vacuo
  7. 7
    その他The residue is recrystallized from isopropyl alcohol

実験手順

A mixture of 174.6 grams (1.15 mole) of 3-phenylpropyl thiol, 158.8 grams (1.15 mole) of p-fluoroacetophenone and 158.8 grams (1.15 mole) of potassium carbonate in 500 ml. of dry dimethylformamide is stirred at its reflux temperature for approximately 24 hours. The reaction mixture is cooled, water added and extracted with methylene chloride. The extract is washed with water, a solution of 2 N sodium hydroxide, dried over anhydrous sodium sulfate and evaporated in vacuo. The residue is recrystallized from isopropyl alcohol to yield the desired p-(3-phenylpropylthio)acetophenone having a m.p. of 76°-8° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04038412uspto-grants-1977_07