反应详情

To a solution of 5-bromo-2-aminopyrimidine (2.0 g, 11.5 mmole) in CH2Cl2 (75 mL) at RT was added 2,6-lutidine (2.7 mL, 23.0 mmole) followed by acetyl chloride (0.99 g, 12.6 mmole). After stirring for 8 hours, the reaction solution was concentrated under vacuum. The remaining residue was dissolved EtOAc (200 mL), washed with H2O (100 mL) and brine, and dried over Na2SO4. Flash chromatography on silica gel (95:5 CHCl3/MeOH) and drying under high vacuum gave the title compound (1.74 g, 70%) as a yellow solid: MS (ES) m/e 217 (M+H)+.

1. concentrationthe reaction solution was concentrated under vacuum
2. dissolutionThe remaining residue was dissolved EtOAc (200 mL)
3. washwashed with H2O (100 mL) and brine
4. dry with materialdried over Na2SO4
5. customFlash chromatography on silica gel (95:5 CHCl3/MeOH) and drying under high vacuum