反应详情

To a solution of 3-(4-(3-(2-(trifluoromethyl)phenyl)ureido)phenyl)-[1,2,4]triazolo[4,3-b]pyridazine-8-carboxylic acid (66H) (38 mg, 0.086 mmol) in anhydrous DMF (1 mL) was added L-valine tert-butyl ester hydrochloride (23.4 mg, 0.11 mmol), EDC (24.7 mg, 0.13 mmol), HOBt (17 mg, 0.13 mmol), followed by DIPEA (45 μL, 0.26 mmol). The reaction mixture was stirred at room temperature for 3 h. Analysis by LC/MS indicated the starting material was consumed. The reaction mixture was partitioned between EtOAc and water, then the separated EtOAc layer was washed with water, saturated aqueous NaHCO3, saturated aqueous NaCl, dried (anhydrous Na2SO4), and concentrated. The obtained crude residue was purified using a silica gel cartridge (12 g) eluting with a gradient of EtOAc (0-100%) in hexanes to afford 33 mg (63%) of the title compound as a yellow solid. HPLC/MS (Method B): retention time=4.04 min, [M+H]+=598.4.

1. customwas consumed
2. customThe reaction mixture was partitioned between EtOAc and water
3. washthe separated EtOAc layer was washed with water, saturated aqueous NaHCO3, saturated aqueous NaCl
4. dry with materialdried (anhydrous Na2SO4)
5. concentrationconcentrated
6. customThe obtained crude residue
7. customwas purified
8. washeluting with a gradient of EtOAc (0-100%) in hexanes