تفاعل #74902

ord-b0a8a49ae46944b3a2df9093aa91678e

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONA mixture of 25 g
  2. 2
    درجة الحرارةreflux temperature
  3. 3
    درجة الحرارةmaintained
  4. 4
    درجة الحرارةat reflux for 16 hours
  5. 5
    workup.ADDITIONTo the mixture is added 50 g
  6. 6
    أخرىwhile collecting water in a Barrett water trap
  7. 7
    workup.ADDITIONThe mixture is then diluted with a mixture of water and benzene
  8. 8
    غسيلThe benzene layer is washed with water
  9. 9
    أخرىIt is collected
  10. 10
    غسيلrinsed with benzene
  11. 11
    أخرىdried
  12. 12
    أخرىto provide a white powder which
  13. 13
    أخرىis recrystallized from ethanol

الإجراء التجريبي

A mixture of 25 g. (0.181 mole) of 3,4-methylenedioxyphenol, 36 g. (0.181 mole) of α-bromoacetophenone and 41.2 g. (0.40 mole) of sodium carbonate in 350 ml. of benzene is heated to its reflux temperature and maintained at reflux for 16 hours. To the mixture is added 50 g. of potassium carbonate, and the mixture is refluxed for an additional 7 days while collecting water in a Barrett water trap. The mixture is then diluted with a mixture of water and benzene. The benzene layer is washed with water, then cold 5 percent sodium hydroxide solution. A precipitate forms in the benzene layer. It is collected, rinsed with benzene and dried to provide a white powder which is recrystallized from ethanol to provide α-(3,4-methylenedioxyphenoxy)acetophenone, m.p. 123°-126° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04174403uspto-grants-1979_11