反应详情

温度

100 °C

Methyl 2-bromoisonicotinate (4 g, 18.52 mmol), 3,4,5-trifluorophenylboronic acid (4.89 g, 27.77 mmol), potassium carbonate (3.84 g, 27.77 mmol) and PdCl2 (dppf) (0.402 g, 0.56 mmol) were mixed in methanol (30 mL) in two separate 20 mL microwave vials. The vials were capped and heated at 100° C. for 10 min in a single node microwave reactor. Water and DCM were added and the phases were separated. The water phase (pH 9) was extracted with DCM and the combined organic phase washed with brine, passed through a phase separator and evaporated to yield a brown solid. The residue was dissolved in DCM and purified by SCX-2 cation exchange chromatography. Methyl 2-(3,4,5-trifluorophenyl)isonicotinate (2.62 g, 52%) was isolated as a slightly yellow solid. MS m/z 268 (M+H)+

1. customseparate 20 mL microwave vials
2. customThe vials were capped
3. additionWater and DCM were added
4. customthe phases were separated
5. extractionThe water phase (pH 9) was extracted with DCM
6. washthe combined organic phase washed with brine
7. customevaporated
8. customto yield a brown solid
9. custompurified by SCX-2 cation exchange chromatography