反应详情

To a mixture of 1-{5-chloro-2-[4-(3,5-dimethylpyridin-2-yl)piperazine-1-carbonyl]phenyl}pyrrolidin-2-one (206 mg) described in Preparation Example 121, (R)-4-methyloxazolidin-2-one (50.6 mg) described in Preparation Example 25, cesium carbonate (228 mg), tris(dibenzylideneacetone)dipalladium (0) chloroform (51.8 mg) and 2-di-tert-butylphosphino-3,4,5,6-tetramethyl-2′,4′,6′-triisopropyl-1,1′-biphenyl (24 mg) was added toluene (1 mL), and the mixture was refluxed for 8 hr. After cooling, water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. After evaporation of the solvent, the residue was purified by column chromatography (ethyl acetate:methanol). The obtained compound was dissolved in ethyl acetate, 4N hydrogen chloride/ethyl acetate (0.13 mL) was added, and the precipitate was collected by filtration to give the title compound (89.3 mg).

1. temperaturethe mixture was refluxed for 8 hr
2. temperatureAfter cooling
3. extractionthe mixture was extracted with ethyl acetate
4. customAfter evaporation of the solvent
5. customthe residue was purified by column chromatography (ethyl acetate:methanol)
6. dissolutionThe obtained compound was dissolved in ethyl acetate
7. addition4N hydrogen chloride/ethyl acetate (0.13 mL) was added
8. filtrationthe precipitate was collected by filtration