反应详情

温度

0 °C

6-Chloropyrimidine-4,5-diamine (Intermediate 88) (90 mg) was added slowly to HI (57%, aq) (2 mL) at 0° C. The reaction mixture was allowed to stir at 0° C. for 30 minutes and then at ambient temperature for 24 hours. NaHCO3 (sat aq.) was added dropwise until the reaction mixture was pH 8. The product was extracted with EtOAc (3×15 mL). The combined organics were dried (MgSO4), filtered and concentrated in vacuo to afford the title compound as a grey solid (144 mg, 98%);

1. waitat ambient temperature for 24 hours
2. extractionThe product was extracted with EtOAc (3×15 mL)
3. dry with materialThe combined organics were dried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated in vacuo