反应详情

120 ml of water and sodium hydroxide (14.00 g, 0.35 mol) were placed in a conical flask and dissolved. 4,4'-Dihydroxybiphenyl (28.00 g, 0.15 mol) was then added and heated to reflux for 2 hours with stirring using a condenser. Dimethyl sulfate (14.5 ml, 0.15 mol) was added dropwise over about 40 minutes. After addition, the mixture was heated while stirring for 2 hours, and then allowed to cool and filtrated. The filter cake was transferred into 700 ml of water, which was then heated to boiling temperature, and filtrated while still keeping warm. The filtrate was kept at 70° C., and 20% hydrochloric acid was added. White precipitation: formed was washed extensively. Recrystallization from ethanol yielded 4'-methoxy-4-hydroxybiphenyl (13.17 g, Yield: 48.0%).

1. dissolutiondissolved
2. temperatureheated
3. temperatureto reflux for 2 hours
4. additionAfter addition
5. temperaturethe mixture was heated
6. stirringwhile stirring for 2 hours
7. temperatureto cool
8. filtrationfiltrated
9. temperaturewas then heated
10. filtrationfiltrated
11. temperaturewhile still keeping warm
12. customwas kept at 70° C.
13. addition20% hydrochloric acid was added
14. customWhite precipitation
15. customformed
16. washwas washed extensively
17. customRecrystallization from ethanol