反应详情

3-Cyano-benzoic acid (1.2 eq), the amine derivative (1 eq), HOBt (1.2 eq), DIEA (1.2 eq) and EDCI.HCl (1.2 eq) were dissolved in dry DMF (0.15 M), under argon. The mixture was stirred at room temperature overnight. DMF is evaporated and saturated NaHCO3 solution was added. Product was extracted with EtOAc, dried over Na2SO4, filtered and evaporated. The crude was purified on reverse phase (H2O 1% TFA/MeCN 1% TFA 100/0, 0/100). MeCN was evaporated. The product was suspended in H2O and basified with saturated NaHCO3 solution until pH=8-9. The aqueous layer was extracted three times with AcOEt. The organic layer was evaporated to give the final compound.

1. customDMF is evaporated
2. additionsaturated NaHCO3 solution was added
3. extractionProduct was extracted with EtOAc
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. customevaporated
7. customThe crude was purified on reverse phase (H2O 1% TFA/MeCN 1% TFA 100/0, 0/100)
8. customMeCN was evaporated
9. extractionThe aqueous layer was extracted three times with AcOEt
10. customThe organic layer was evaporated