反应详情

温度

105 °C

A mixture of 3-bromobenzonitrile (910 mg), Pd(Ph3P)4 (290 mg), (Me3Sn)2 (1.64 g) and dioxane (20 mL) was sealed under argon in a pressure tube. The tube was then heated at 100-110° C. for 3 hours with stirring and another 15 hours at 80° C. To the reaction mixture was added 1-bromo-3-methylbenzene (940 mg), Pd(PPh3)4 (290 mg) and dioxane (5 mL) under argon. The sealed tube was heated at 135-140° C. with stirring for two days. The catalyst was filtered off and the filtrate was poured into water and extracted with ethyl acetate (3×). The organic layer was washed with brine, dried over Mg2SO4, concentrated and purified on silica gel column (ethyl acetate/hexane, 1:3) to afford 0.64 g of 3-(3-cyanophenyl)-1-methylbenzene.

1. customwas sealed under argon in a pressure tube
2. temperatureThe sealed tube was heated at 135-140° C.
3. stirringwith stirring for two days
4. filtrationThe catalyst was filtered off
5. additionthe filtrate was poured into water
6. extractionextracted with ethyl acetate (3×)
7. washThe organic layer was washed with brine
8. dry with materialdried over Mg2SO4
9. concentrationconcentrated
10. custompurified on silica gel column (ethyl acetate/hexane, 1:3)