反应详情

A mixture of 1.0 g (2.2 mmol) of 1-(1,1-dimethylethyl)-5-hydroxy-4-(3-iodo-2-methyl-4-methylsulfonylbenzoyl)pyrazole, 0.541 g (3.3 mmol) of 4-ethoxyphenylboronic acid, 0.607 g (4.4 mmol) of potassium carbonate, 0.025 g (0.11 mmol) of palladium(II) acetate, 0.100 g (0.33 mmol) of tri-o-tolylphosphine, 25 mL of acetonitrile, and 3 mL of water was heated at reflux with stirring for 15 min. The resulting mixture was cooled and diluted with water. The mixture obtained was extracted with ether and acidified with concentrated aqueous hydrochloric acid. The yellow precipitate that formed was collected by filtration and recrystallized by dissolving in dichloromethane and then adding hexane to obtain 800 mg (80 percent of theory) of the title compound as a white solid melting at 110° C.

1. temperaturewas heated
2. temperatureat reflux
3. temperatureThe resulting mixture was cooled
4. customThe mixture obtained
5. extractionwas extracted with ether
6. customThe yellow precipitate that formed
7. filtrationwas collected by filtration
8. customrecrystallized
9. dissolutionby dissolving in dichloromethane