反应详情

To a suspension of 2-({2-chloro-7-[(4-methylphenyl)sulfonyl]-7H-pyrrolo[2,3-d]pyrimidin-4-yl}amino)-6-fluorobenzamide (5.0 g, 10.87 mmol), 1-[(dimethylamino)acetyl]-6-(methyloxy)-1,2,3,4-tetrahydro-7-quinolinamine (3.44 g, 13.05 mmol), and potassium iodide (0.090 g, 0.544 mmol) in trifluroethanol (250 ml) was added 4M HCl/dioxane (10.87 ml, 43.5 mmol). The reaction was heated overnight in a pressure vessel equipped with a threaded teflon cap. The reaction was diluted with THF (300 ml) and washed with saturated NaHCO3 (300 ml). The organic layer was removed, concentrated on rotovap, solids triturated from ethyl acetate/hexanes, and dried under house vacuum prior to next step to afford 5-{[1-(N,N-dimethylglycyl)-6-(methyloxy)-1,2,3,4-tetrahydro-7-quinolinyl]amino}-8-fluoro-3-[(4-methylphenyl)sulfonyl]pyrrolo[2′,3′:4,5]pyrimido[6,1-b]quinazolin-7(3H)-one (5.0 g, 68%). ESIMS (M+H)+=670.

1. temperatureThe reaction was heated overnight in a pressure vessel
2. customcap
3. washwashed with saturated NaHCO3 (300 ml)
4. customThe organic layer was removed
5. concentrationconcentrated on rotovap, solids
6. customtriturated from ethyl acetate/hexanes
7. customdried under house vacuum