反应详情

To a solution 2-(4-bromophenyl)-3-{4-[2-(2,6-dichloro-4-methylphenoxy)ethoxy]phenyl}propanenitrile (1 eq.) from step 1,2-chlorophenylboronic acid (2 eq.) in n-propanol:dioxane (1:2; 0.17M) at room temperature was added palladium acetate/triphenyl phosphine (1:3; 0.05 eq.) and aqueous Na2CO3 (2M; 4 eq.). The mixture was stiffed 30 min at 150° C. in microwave (Smith Creator; Personal Chemistry), cooled to room temperature, poured in water and extracted with EtOAc. The organic extract was washed with water, brine, dried over MgSO4 filtered and concentrated. Purification by column chromatography on silica gel, eluting with Hex/EtOAc 5% afforded the desired compound.

1. extractionextracted with EtOAc
2. extractionThe organic extract
3. washwas washed with water, brine
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated
7. customPurification by column chromatography on silica gel
8. washeluting with Hex/EtOAc 5%