反应详情

25.0 g of crude 4-(4-tert-butyl-phenyl)-2-(1-ethylcyclo-hexylmethylene)-indan-1-one (GC: ˜83% purity) are dissolved in 250 ml of ethyl acetate in a flask with gas inlet and stirrer. 1.75 g of palladium on activated carbon (10 wt-% palladium) are added. The system is evacuated and refilled with argon three times to remove oxygen and then evacuated and refilled with hydrogen three times. The stirrer is started and the reaction mixture is vigorously stirred to help the diffusion of hydrogen gas into the liquid reaction mixture. The hydrogen uptake is monitored and stirring is continued until the hydrogen uptake ceases. Filtering the crude reaction mixture over a paper filter and removing the solvent in a vacuum leaves crude 4-(4-tert-butyl-phenyl)-2-(1-ethyl-cyclohexylmethyl)-indan-1-one (yield 24.4 g, GC: ˜82% purity). The obtained crude product was used without further purification for the subsequent reduction/elimination-sequence.

1. customThe system is evacuated
2. additionrefilled with argon three times
3. customto remove oxygen
4. customevacuated
5. additionrefilled with hydrogen three times
6. custominto the liquid reaction mixture
7. stirringstirring
8. filtrationFiltering the crude
9. customreaction mixture over a paper
10. filtrationfilter
11. customremoving the solvent in a vacuum