반응 #74902

반응 방정식

potassium carbonate

3,4-methylenedioxyphenol

α-bromoacetophenone

sodium carbonate

→

α-(3,4-methylenedioxyphenoxy)acetophenone

용매

benzene

반응 조건

후처리

1. 1
   workup.ADDITIONA mixture of 25 g
2. 2
   온도reflux temperature
3. 3
   온도maintained
4. 4
   온도at reflux for 16 hours
5. 5
   workup.ADDITIONTo the mixture is added 50 g
6. 6
   기타while collecting water in a Barrett water trap
7. 7
   workup.ADDITIONThe mixture is then diluted with a mixture of water and benzene
8. 8
   세척The benzene layer is washed with water
9. 9
   기타It is collected
10. 10
    세척rinsed with benzene
11. 11
    기타dried
12. 12
    기타to provide a white powder which
13. 13
    기타is recrystallized from ethanol

실험 절차

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.

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