反应详情

温度

80 °C

2-Fluoro-4-methylphenylamine (1.10 equivalents), palladium (II) acetate (0.10 equivalents), rac-2,2-bis(diphenylphosphino)-1,1′-binaphthyl (0.15 equivalents), and cesium carbonate (1.50 equivalents) are added to a solution of 4-chloro-1,3,8-trimethyl-1H,6H-pyrido[2,3-d]pyridazine-2,5-dione (1.00 equivalent) in toluene in a sealed vial. After stirring 10 minutes, the mixture is heated to 80° C. After 24 hours, the reaction mixture is cooled to room temperature and diluted with EtOAc. The resulting precipitate is filtered and washed with EtOAc. The filtrate is diluted with EtOAc and washed with water. The aqueous layer is reextracted with EtOAc. The combined organic layers are washed with brine, dried (Na2SO4) and concentrated. Purification by flash column chromatography gives the desired product.

1. waitAfter 24 hours
2. temperaturethe reaction mixture is cooled to room temperature
3. filtrationThe resulting precipitate is filtered
4. washwashed with EtOAc
5. additionThe filtrate is diluted with EtOAc
6. washwashed with water
7. washThe combined organic layers are washed with brine
8. dry with materialdried (Na2SO4)
9. concentrationconcentrated
10. customPurification by flash column chromatography