反应详情

A solution of dimethyl 5-iodoisophthalate (6 g, 18.75 mmol, 1 eq.), 4-cyanophenylboronic acid (2.95 g, 19.68 mmol, 1.05 eq.) and Na2CO3 (7.95 g, 74.98 mmol, 4 eq.) in 400 mL of MeOH was degassed by 4 thaw-freeze-pump cycles. Then 1.3 g of 5% Pd/C was added and nitrogen gas was bubbled through the solution for 10 min. The reaction under stirring was carried out at 80° C. for 1 h. Then, the mixture was filtered and washed with EtOH and CH2Cl2. All organic solvents were removed under vacuum and aqueous layer was extracted 4 times with CH2Cl2, the recombined organic layer were washed once with H2O, dried over MgSO4, filtered and evaporated under vacuum. An off-white solid was obtained with 85% yield.

1. customnitrogen gas was bubbled through the solution for 10 min
2. customThe reaction
3. filtrationThen, the mixture was filtered
4. washwashed with EtOH and CH2Cl2
5. customAll organic solvents were removed under vacuum and aqueous layer
6. extractionwas extracted 4 times with CH2Cl2
7. washthe recombined organic layer were washed once with H2O
8. dry with materialdried over MgSO4
9. filtrationfiltered
10. customevaporated under vacuum
11. customAn off-white solid was obtained with 85% yield