反应详情

A solution of benzoic acid N′-[2-(2-bromo-phenylsulfanyl)-acetyl]-N′-isopropyl-hydrazide (50 mg, 0.123 mmol) in DME (4 ml)/2M Na2CO3 (0.645 ml, 1.29 mmoles) was treated with 2,3-dimethylphenylboronic acid (36.9 mg, 0.246 mmol) and Pd[PPh3]4 (70.2 mg, 0.061 mmol) for 65 hours at 90° C. The reaction mixture was partitioned between water and DCM. The organic layer was washed with brine, dried over sodium sulfate, filtered, and concentrated. The crude was adsorbed on silica and purified on a silica gel column with a 20-50% ethyl acetate/hexane gradient. Further purification by RP HPLC afforded the product (8.5 mg, 16.4%). MS m/e 433.24 (M+H+)

1. customThe reaction mixture was partitioned between water and DCM
2. washThe organic layer was washed with brine
3. dry with materialdried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. custompurified on a silica gel column with a 20-50% ethyl acetate/hexane gradient
7. customFurther purification by RP HPLC