反应详情

温度

50 °C

4.83 g of sodium borohydride and 39.1 g of 2-isopropyl-7-(4′-tert-butylphenyl)-1-indanone together with 11.8. ml of toluene are placed in a reaction vessel. At 50° C., 22.5 ml of methanol are slowly added and the reaction mixture is stirred for 6 hours at 50° C. After cooling to room temperature, 50 ml of 2N sulfuric acid are added and the mixture is stirred vigorously for another 30 minutes. The mixture is subsequently transferred to a separating funnel, the phases are separated and the aqueous phase is shaken twice with a total of 60 ml of 2N sulfuric acid. The organic phases are combined and dried over magnesium sulfate. The solvent of the reaction mixture is removed virtually completely and 200 ml of toluene and 0.4 g of p-toluenesulfonic acid are subsequently added to the residue. Water is distilled from the reaction mixture by heating for 1.5 hours on a water separator until reaction is complete. The reaction mixture is subsequently washed once with 100 ml of saturated sodium hydrogen carbonate solution and dried over magnesium sulfate. After separating off the magnesium sulfate, the residue is dried in an oil pump vacuum. This gives 35.7 g of 2-isopropyl-4-(4′-tert-butylphenyl)indene (total yield: 96%).

1. temperatureAfter cooling to room temperature
2. stirringthe mixture is stirred vigorously for another 30 minutes
3. customThe mixture is subsequently transferred to a separating funnel
4. customthe phases are separated
5. stirringthe aqueous phase is shaken twice with a total of 60 ml of 2N sulfuric acid
6. dry with materialdried over magnesium sulfate
7. customThe solvent of the reaction mixture is removed virtually completely
8. addition200 ml of toluene and 0.4 g of p-toluenesulfonic acid are subsequently added to the residue
9. distillationWater is distilled from the reaction mixture
10. temperatureby heating for 1.5 hours on a water separator until reaction
11. washThe reaction mixture is subsequently washed once with 100 ml of saturated sodium hydrogen carbonate solution
12. dry with materialdried over magnesium sulfate
13. customAfter separating off the magnesium sulfate
14. customthe residue is dried in an oil pump vacuum