反应详情

step 2—A microwave vial was charged with 64 (903 mg, 3.00 mmol), 2-benzyloxy-3-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)pyridine (1.12 g, 3.60 mmol), Pd(PPh3)4 (173 mg, 0.15 mmol), Na2CO3 (950 mg, 9.00 mmol), MeOH (10 mL) and DCM (3 mL). The vial was sealed and irradiated at 115° C. for 30 min in microwave synthesizer. The reaction was quenched with H2O and extracted with DCM. The combined organics were dried (MgSO4) and concentrated under reduced pressure. The residue was purified by SiO2 chromatography eluting with a EtOAc/hexane gradient (10% to 20% EtOAc) to afford 964 mg (80%) of 2-(2-benzyloxypyridin-3-yl)-4-tert-butyl-5-methoxybenzoic acid methyl ester (66) as a light yellow solid.

1. customThe vial was sealed
2. customirradiated at 115° C. for 30 min in microwave synthesizer
3. customThe reaction was quenched with H2O
4. extractionextracted with DCM
5. dry with materialThe combined organics were dried (MgSO4)
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified by SiO2 chromatography
8. washeluting with a EtOAc/hexane gradient (10% to 20% EtOAc)