反应详情

A solution of benzoic acid N′-[2-(2-bromo-4-fluoro-phenoxy)-acetyl]-N′-isopropyl-hydrazide (50 mg, 0.122 mmol) in DME (3 ml)/2M Na2CO3 (215 uL, 0.427 mmol) was treated with 4-fluorobenzeneboronic acid (26 mg, 0.183 mmol) and Pd[PPh3]4 (28 mg, 0.0244 mmol) for 12 hours at 90° C. The reaction mixture was partitioned between water and ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate, filtered, and concentrated. The crude was absorbed on silica and purified on a silica gel column with a 30-50% ethyl acetate/hexanes gradient to afford the product as a beige solid (42 mg, 81%). LC-MS m/e 425.28 (M+H+)

1. customThe reaction mixture was partitioned between water and ethyl acetate
2. washThe organic layer was washed with brine
3. dry with materialdried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. customThe crude was absorbed on silica
7. custompurified on a silica gel column with a 30-50% ethyl acetate/hexanes gradient