反应详情

Under argon, in a heat-dried apparatus, 7.4 mg of Pd(OAc)2, 22 mg of di-tert-butyl(2′-methylbiphenyl-2-yl)phosphine and 0.78 g of K3PO4 in 4.8 ml of air-free dioxane are introduced as initial charge. 203 mg of 5,5-dimethylpyrrolidine-2,4-dione and 659 mg of 3-(4-chlorophenyl)-6-methylbromobenzene are added and the mixture is stirred for 16 hours under reflux. The mixture is then left to cool to room temperature, diluted with ca. 6 ml of methanol and filtered, and the filter residue is after-washed with ca. 3 ml of MeOH. The combined filtrates are concentrated by evaporation on a rotary evaporator. The residue is taken up in ca. 6 ml of water and rendered weakly acidic using 1 N hydrochloric acid. The precipitated solid is filtered off with suction and washed with ca. 3 ml of water. It is then washed from the filter with acetone and the filtrate is concentrated by evaporation. This gives 0.597 g of solid. Reversed-phase separation with water/acetonitrile (gradient) gives 93 mg (14% of theory) with a purity of 98.6% according to HPLC/MS.

1. additionas initial charge
2. temperatureunder reflux
3. waitThe mixture is then left
4. filtrationfiltered
5. washthe filter residue is after-washed with ca. 3 ml of MeOH
6. concentrationThe combined filtrates are concentrated by evaporation on a rotary evaporator
7. filtrationThe precipitated solid is filtered off with suction
8. washwashed with ca. 3 ml of water
9. washIt is then washed from the
10. filtrationfilter with acetone
11. concentrationthe filtrate is concentrated by evaporation
12. customReversed-phase separation with water/acetonitrile (gradient)
13. customgives 93 mg (14% of theory) with a purity of 98.6%