反应详情

To a solution of Compound (8) (51.4 mg, 0.148 mmol) in THF (2 mL) was added phosphorus tribromide (0.2 mL). The reaction mixture was allowed to stir at room temperature for 5 minutes then quenched with saturated sodium bicarbonate solution and extracted with dichloromethane. The combined organic layers were dried over NaSO3 and evaporated to give Compound (9) as a white solid. The crude mixture was used in the next step without further purification. The identity of the product was verified by LCMS. LCMS: m/z for C16H19N5O4++H observed 346.1 at 1.69 minutes of a 3.5 minute run, gradient 5-95% CH3CN in H2O. LCMS: m/z for C16H18BrN5O3++H observed 408.0 and 410.1 at 2.03 minutes of a 3.5 minute run, gradient 5-95% CH3CN in H2O (C18 column).

1. customthen quenched with saturated sodium bicarbonate solution
2. extractionextracted with dichloromethane
3. dry with materialThe combined organic layers were dried over NaSO3
4. customevaporated