반응 #346839

ord-4cec5fb0ee97485c9bd8bce822d61aa2

반응 방정식

CN(C)C=O
dimethylformamide
SCCCc1ccccc1
3-phenylpropyl thiol
CC(=O)c1ccc(F)cc1
p-fluoroacetophenone
O=C([O-])[O-].[K+].[K+]
potassium carbonate
CC(=O)c1ccc(SCCCc2ccccc2)cc1
p-(3-phenylpropylthio)acetophenone

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도reflux temperature for approximately 24 hours
  2. 2
    온도The reaction mixture is cooled
  3. 3
    추출extracted with methylene chloride
  4. 4
    세척The extract is washed with water
  5. 5
    건조a solution of 2 N sodium hydroxide, dried over anhydrous sodium sulfate
  6. 6
    기타evaporated in vacuo
  7. 7
    기타The residue is recrystallized from isopropyl alcohol

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04038412uspto-grants-1977_07