反应详情

A suspension of 6-bromo-4-((4,4-dimethylpyrrolidin-3-yl)amino)pyrrolo[1,2-b]pyridazine-3-carboxamide hydroiodide (97 mg, 0.25 mmol) in DCM (3 mL), was added DIPEA (0.16 mL, 0.87 mmol) and methanesulfonyl chloride (0.04 mL, 0.5 mmol). The mixture was stirred at rt overnight. The reaction was quenched with water, extracted by dichloromethane, washed with hydrochloride (0.5N), aq. sodium bicarbonate and brine. The organic layer was dried over sodium sulfate and concentrated. The residue was triturated in ether then filtered to give (+/−)-6-bromo-4-(4,4-dimethyl-1-(methylsulfonyl)pyrrolidin-3-ylamino)pyrrolo[1,2-b]pyridazine-3-carboxamide (92 mg, 86%). MS (ES+) m/z: 431.99 (M+H).

1. customThe reaction was quenched with water
2. extractionextracted by dichloromethane
3. washwashed with hydrochloride (0.5N), aq. sodium bicarbonate and brine
4. dry with materialThe organic layer was dried over sodium sulfate
5. concentrationconcentrated
6. customThe residue was triturated in ether
7. filtrationthen filtered