反应详情

A mixture of INTERMEDIATE 9 (1.0 g, 1.93 mmol), 2-fluoro-5-nitro phenyl boronic acid (0.51 g, 2.74 mmol), tetrakis(triphenylphosphine) palladium (223 mg, 10% mol) and Na2CO3 (410 mg, 3.86 mmol) in 14 mL of water/EtOH/toluene (1:2:4) was heated at reflux for 2 h. The solvents were removed. Water (20 mL) was added. The organic was extracted with CH2Cl2 (3×10 mL). The combined CH2Cl2 layers were washed with brine, and dried (Na2SO4). The title compound was obtained after flash chromatography using CH2Cl2/hexane (8:2) as the eluant. LCMS M+H 578.30.

1. temperaturewas heated
2. temperatureat reflux for 2 h
3. customThe solvents were removed
4. additionWater (20 mL) was added
5. extractionThe organic was extracted with CH2Cl2 (3×10 mL)
6. washThe combined CH2Cl2 layers were washed with brine
7. dry with materialdried (Na2SO4)