反应详情

In a three necked round bottom flask (equipped with a condensor, additional funnel and mechanical stirrer) was added 15.2 g of a combination of Raney Nickel and Ni supported on silica. (50:50). 100 ml of a mixture of 50:50 ethanol:water was added and the reaction was heated at reflux conditions. 15.2 g of 2,4-dihydroxy acetophenone in 100 ml of water:ethanol and 10 ml of acetic acid was placed in the additional funnel and slowly added to the mixture (dropwise). The reaction was filtered through a milipore filter to give a pale yellow solution. Concentration of this solution in vacuo gave a solid. This solid was crystalized from 1,2-dichloroethane to give 4-ethyl resorcinol in 80% isolated yield. The unreacted 2,4-dihydroxy acetophenone was recovered (−17%) form the reaction mixture and was recycled. The structure of 4-ethyl resorcinol and 2,4-dihydroxy acetophenone were characterized by NMR, Gas Chromatography, IR and Mass spectroscopy

1. customIn a three necked round bottom flask (equipped with a condensor, additional funnel and mechanical stirrer)
2. temperaturethe reaction was heated
3. temperatureat reflux conditions
4. additionslowly added to the mixture (dropwise)
5. filtrationThe reaction was filtered through a milipore
6. filtrationfilter
7. customto give a pale yellow solution
8. customConcentration of this solution in vacuo gave a solid
9. customThis solid was crystalized from 1,2-dichloroethane