反应详情

温度

-25 °C

7-(1,4-oxazepan-4-ylmethyl)pyrrolo[2,1-f][1,2,4]triazin-4-amine (1.90 g, 7.68 mmol) was suspended in chloroform (76 mL). The solution was cooled to −20 to −30° C. 1,3-dibromo-5,5-dimethylimidazolidine-2,4-dione ( 989 g, 3.46 mmol) was added. The reaction was maintained at −20° C. for 20 minutes then warmed to room temperature. An LC taken at that time showed the reaction to be essentially complete. The reaction was then quenched by the addition of saturated aqueous sodium sulfite. The resultant slurry was partitioned between ethyl acetate (300 mL) and saturated bicarbonate (100 mL). The organic layer was washed (3×100 mL) with bicarb then dried with Na2SO4 and concentrated under vacuum.

1. temperatureThe reaction was maintained at −20° C. for 20 minutes
2. temperaturethen warmed to room temperature
3. customthe reaction
4. customThe reaction was then quenched by the addition of saturated aqueous sodium sulfite
5. customThe resultant slurry was partitioned between ethyl acetate (300 mL) and saturated bicarbonate (100 mL)
6. washThe organic layer was washed (3×100 mL) with bicarb
7. dry with materialthen dried with Na2SO4
8. concentrationconcentrated under vacuum