Reaktion #60880
ord-36d650d9bef54b7e970ce0e95d3a1b3e
Reaktionsgleichung
Reagenzien
Keine
Reaktionsbedingungen
Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1workup.WAITat ambient temperature for 24 hours
- 2ExtraktionThe product was extracted with EtOAc (3×15 mL)
- 3TrocknenThe combined organics were dried (MgSO4)
- 4Filtrationfiltered
- 5Einengenconcentrated in vacuo
Vorschrift
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%);