反应详情

Methyl 2-bromo-6-fluorobenzoate (2, 11.29 g, 48.5 mmol), cyclopropylboronic acid (6.24 g, 72.7 mmol), K3PO4 (30.85 g, 145.4 mmol) and Pd(PPh3)4 (2.80 g, 2.4 mmol) were mixed under argon in a degassed mixture of toluene and water (20:1, 160 mL). The resulting brown suspension was heated at reflux for 2.5 h, cooled, filtered through Celite, and evaporated. The residue was partitioned between ethyl acetate (150 mL) and brine (150 mL). The layers were separated and organic layer was dried over magnesium sulfate and evaporated. The oily residue was suspended in hexane and the solid was removed by filtration. Evaporation of the filtrate afforded the title compound (9.30 g, 47.9 mmol, 99%) as a light brown oil.

1. temperatureThe resulting brown suspension was heated
2. temperatureat reflux for 2.5 h
3. temperaturecooled
4. filtrationfiltered through Celite
5. customevaporated
6. customThe residue was partitioned between ethyl acetate (150 mL) and brine (150 mL)
7. customThe layers were separated
8. dry with materialorganic layer was dried over magnesium sulfate
9. customevaporated
10. customthe solid was removed by filtration
11. customEvaporation of the filtrate