反应详情

温度

90 °C

5.0 g (20.7 mmol) of 7-bromo-1-benzofuran-2-carboxylic acid (Example 29A) and 3.78 g (24.9 mmol) of 2-methoxyphenylboronic acid are introduced into 50 ml of DMF. Addition of 31.1 ml of 2 M sodium carbonate solution and 1.2 g (1.04 mmol) of Pd(PPh3)4 is followed by heating to 90° C. After 18 h, the solvent is distilled out. The residue is partitioned between 1N hydrochloric acid and ethyl acetate and extracted three times with 200 ml of ethyl acetate each time. The organic phase is dried over sodium sulphate and concentrated in vacuo. The residue is purified by flash chromatography (silica gel, mobile phase: dichloromethane/methanol/acetic acid 100:10:1). Concentration and drying under high vacuum result in 2.97 g (53.2% of theory) of the title compound.

1. distillationthe solvent is distilled out
2. customThe residue is partitioned between 1N hydrochloric acid and ethyl acetate
3. extractionextracted three times with 200 ml of ethyl acetate each time
4. dry with materialThe organic phase is dried over sodium sulphate
5. concentrationconcentrated in vacuo
6. customThe residue is purified by flash chromatography (silica gel, mobile phase: dichloromethane/methanol/acetic acid 100:10:1)
7. concentrationConcentration
8. customdrying under high vacuum