反应详情

A mixture of 46.33 mg (0.1 mmol) cis-2,6-dimethyl-piperazine-1,4-dicarboxylic acid 1-(3-bromo-2,6-difluoro-benzyl) ester 4-tert-butyl ester, 16.71 mg (0.11 mmol) 2-methoxyphenylboronic acid, 3.65 mg (0.005 mmol) dichloro(1,1′-bis(diphenylphosphino) ferrocene)palladium (II) dichloromethane adduct and 0.11 ml of a 2M Na2CO3 aq. solution in 1.2 ml dioxane was heated for 17 h to 85° C. The mixture was filtered and 0.15 ml 4N HCl in dioxane was added and the mixture heated for 3 h to 65° C. After cooling to ambient temperature 0.2 ml triethylamine and water were added to dissolve the mixture. The solution was subjected to reversed phase preparative HPLC eluting with a water/acetonitrile gradient to yield after evaporation of the solvents 28.2 mg (66%) of the title compound. MS (ISP): 391 MH+

1. temperaturewas heated for 17 h to 85° C
2. filtrationThe mixture was filtered
3. addition0.15 ml 4N HCl in dioxane was added
4. temperaturethe mixture heated for 3 h to 65° C
5. additionwere added
6. dissolutionto dissolve the mixture
7. washeluting with a water/acetonitrile gradient
8. customto yield
9. customafter evaporation of the solvents 28.2 mg (66%) of the title compound