反应详情

温度

90 °C

To a solution of 2-chloro-4-(3-chloro-4-fluoro-phenyl)-6-[4-(3-trifluoromethyl-pyridin-2-yl)-piperazin-1-yl]-pyrimidine (259 mg, 0.55 mmol), 3-oxo-piperazine-1-carboxylic acid tert-butyl ester (prepared essentially as described by Kane and Carr (1980) Teit. Lett. 21:3019-20; 132 mg, 0.66 mmol) and Cs2CO3 (250 mg, 0.77 mmol) in dioxane, add 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (19 mg, 0.03 mmol). Purge the reaction mixture for 10 minutes with nitrogen gas and then add Pd2(dba)3 (10 mg, 0.011 mmol). After purging with nitrogen gas for an additional 5 minutes, heat the mixture at 90° C. for 16 hours under nitrogen atmosphere. Filter the mixture through celite and concentrate under reduced pressure to give the title compound.

1. customPurge the reaction mixture for 10 minutes with nitrogen gas
2. customAfter purging with nitrogen gas for an additional 5 minutes
3. filtrationFilter the mixture through celite and
4. concentrationconcentrate under reduced pressure