反应详情

温度

75 °C

A mixture of 27.4 g (140 mmol) of 5-bromo-2-methylbenzonitrile, 19.5 g (160 mmol) of dihydroxyphenylborane, 629 mg (2.8 mmol) of palladium acetate (II), 45.1 g (140 mmol) of tetrabutylammonium bromide, 48.4 g (350 mmol) of potassium carbonate and 280 ml of water was stirred at 75° C. for 11 hours under nitrogen flow. To the reaction solution was added chloroform, the organic layer was washed with water, dried over anhydrous magnesium sulfate, then, concentrated. The residue was re-crystallized from methanol to give 19.9 g (99.9 mmol) of 2-methyl-5-phenylbenzonitrile.

1. washthe organic layer was washed with water
2. dry with materialdried over anhydrous magnesium sulfate
3. concentrationconcentrated
4. customThe residue was re-crystallized from methanol