反应详情

20.6 g (73.0 mmol) methyl (E)-2-acetylamino-3-(4-amino-3-chloro-5-methyl-phenyl)-acrylate, 0.445 g (0.90 mmol) bis(1,5-cyclooctadiene)-di-rhodium(I)-dichloride, 0.744 g (1.8 mmol) 1,3-bis(diphenylphosphino)-propane were dissolved in 400 ml degassed methanol and 12 ml degassed triethylamine and then hydrogenated at ambient temperature under 3 bar hydrogen pressure. The reaction mixture was evaporated down under reduced pressure and taken up in ethyl acetate. The insoluble precipitate was removed by suction filtering and the filtrate was evaporated down under reduced pressure. The residue was purified by column chromatography.

1. customdegassed methanol and 12 ml
2. customdegassed triethylamine
3. customhydrogenated at ambient temperature under 3 bar hydrogen pressure
4. customThe reaction mixture was evaporated down under reduced pressure
5. customThe insoluble precipitate was removed by suction
6. filtrationfiltering
7. customthe filtrate was evaporated down under reduced pressure
8. customThe residue was purified by column chromatography