反应详情

温度

130 °C

A degassed mixture of 3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridin-2-amine (2.4 g, 10.91 mmol), tert-butyl 4-bromo-2-fluorobenzoate (3.30 g, 12.00 mmol), Pd(PPh3)4 (0.63 mg, 0.0.545 mmol), 2.0 M Na2CO3aqueous solution (10.91 mL) in n-butanol (26 mL) was microwave heated to 130° C. for 10 min. The reaction was diluted with ethyl acetate (30 mL), and then washed with water (10 mL) and brine (10 mL). The organics were dried over sodium sulfate, filtered, concentrated, and then purified by flash chromatography (10-60% ethyl acetate/heptane eluent) to provide tert-butyl 4-(2-aminopyridin-3-yl)-2-fluorobenzoate (1.35 g, 43% yield). LCMS (m/z): 289.4 (MH+), 0.67 min.

1. washwashed with water (10 mL) and brine (10 mL)
2. dry with materialThe organics were dried over sodium sulfate
3. filtrationfiltered
4. concentrationconcentrated
5. custompurified by flash chromatography (10-60% ethyl acetate/heptane eluent)