反应详情

To a solution of N-hydroxy-morpholine-4-carboxamidine (Example 419A) (20.2 mg, 0.13 mmol) and Hunig's base (45 μl, 0.26 mmol) in DMF (1 ml) at −5° C. was added a solution of 3-cyano-5-methyl-4-(4-phenoxy-phenylamino)-pyrrolo[1,2-b]pyridazine-6-carbonyl chloride (Example 412B) (51 mg, 0.12 mmol) in DMF (1 ml) via syringe. The reaction mixture was warmed to rt, after 20 min, diluted with EtOAc, poured into water (50 ml), extracted with EtOAc (2×50 ml). The combined extracts were dried with Na2SO4, concentrated in vacuo and purified by prep. TLC to give the title compound (23 mg, 37%) (5% MeOH—CHCl3). It has a retention time of 5.79 min (standard LC1 method, 8 min run). LCMS Found: (M+H)+=512.2.

1. extractionextracted with EtOAc (2×50 ml)
2. dry with materialThe combined extracts were dried with Na2SO4
3. concentrationconcentrated in vacuo
4. custompurified by prep