反应详情

温度

140 °C

To a flask equipped with a stirrer, dropping funnel, condenser and gas inlet tube maintained under a nitrogen atmosphere, there is added 50 g. (0.89) moles of potassium hydroxide in one liter of 2-methoxyethanol. Stirring is initiated and 100 g. (0.79 mole) of anhydrous phloroglucinol is added in three portions, followed by the addition of 100 g. (0.80 mole) of 1-acetyl-cyclohexene while maintaining the temperature at 50° C. The resulting solution is refluxed at 140° C. for 4 hours. After cooling there is then added gradually 53.6 g. of acetic acid while obtaining a pH of approximately 7. The solvent is then removed in vacuo, and the residue is further heated in an oil bath at 70° C., to obtain a viscous residue. The resulting residue is dissolved in ethyl acetate and water washed twice with water, dried over anhydrous sodium sulfate, filtered and evaporated in vacuo to obtain a brown solid. The resulting solid is recrystallized from ethyl acetate/cyclohexane to give 2,4-dihydroxy-4b,5,6,7,8,8a,9,10-octahydro-9-oxo-phenanthrene; m.p. 220°-223° C.

1. customTo a flask equipped with a stirrer
2. temperaturemaintained under a nitrogen atmosphere
3. additionthere is added 50 g
4. additionfollowed by the addition of 100 g
5. temperatureAfter cooling there
6. additionis then added gradually 53.6 g
7. customThe solvent is then removed in vacuo
8. temperaturethe residue is further heated in an oil bath at 70° C.
9. customto obtain a viscous residue
10. washwater washed twice with water
11. dry with materialdried over anhydrous sodium sulfate
12. filtrationfiltered
13. customevaporated in vacuo
14. customto obtain a brown solid
15. customThe resulting solid is recrystallized from ethyl acetate/cyclohexane