反应详情

To a solution of 3,3,3-trifluoropropionic acid (2.07 mmole) in DCM (10 mL), was added EDCI HCl (3.02 mmole) and HOBt (2.07 mmole). The solution was stirred at RT for 0.5 hour followed by addition of 3-hydrazinyl-6-(4-phenoxyphenyl)pyridazine A, prepared as disclosed in Example 3, (2.07 mmole) in 30 mL of DCM and EDIPA ((7.24 mmole). The coupling reaction will also work with 1,3-dicyclohexylcarbodiimide and DCM as a solvent or EDCI HCl and methanol as a solvent. The resulting reaction mixture was stirred at RT overnight. The mixture was diluted with saturated aqueous NaHCO3. The organic extract was washed with H2O and dried over Na2SO4 and then evaporated in vacuo. The crude product was purified with prep TLC eluting with 5% methanol and dichloromethane mixture to give B.

1. customprepared
2. customThe coupling reaction
3. customThe resulting reaction mixture
4. stirringwas stirred at RT overnight
5. extractionThe organic extract
6. washwas washed with H2O
7. dry with materialdried over Na2SO4
8. customevaporated in vacuo
9. customThe crude product was purified with prep TLC
10. washeluting with 5% methanol and dichloromethane mixture
11. customto give B