反应详情

温度

85 °C

Stir a solution of 4.84 g (14.2 mmol) of methyl 3-bromo-4-iodobenzoate (J. Med. Chem., 1999, 42, 4088) and 3.88 g (21.29 mmol) of 2,6-dimethoxyphenyl boronic acid in 120 mL of DMF and 14.2 mL of a 2M aqueous solution of caesium carbonate for 15 minutes under argon, then add 984 mg (0.85 mmol) of Pd(PPh3)4 and heat for 2.5 h at 85° C. After concentration under reduced pressure, distribute the residue obtained in 600 mL of a 1:1 DCM/water mixture. Wash the organic phase with 100 mL of water, dry over MgSO4 and concentrate at reduced pressure. Purify the residue obtained by silica gel column chromatography, eluting with a heptane/EtOAc gradient from 0 to 10% of EtOAc. After concentration under reduced pressure, we obtain 2.79 g of methyl 2-bromo-2′,6′-dimethoxybiphenyl-4-carboxylate in the form of oil.

1. concentrationAfter concentration under reduced pressure
2. customobtained in 600 mL of a 1:1 DCM/water mixture
3. washWash the organic phase with 100 mL of water
4. dry with materialdry over MgSO4
5. concentrationconcentrate at reduced pressure
6. customPurify the residue
7. customobtained by silica gel column chromatography
8. washeluting with a heptane/EtOAc gradient from 0 to 10% of EtOAc
9. concentrationAfter concentration under reduced pressure, we