تفاعل #60880
ord-36d650d9bef54b7e970ce0e95d3a1b3e
معادلة التفاعل
الكواشف
لا شيء
ظروف التفاعل
درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1workup.WAITat ambient temperature for 24 hours
- 2استخلاصThe product was extracted with EtOAc (3×15 mL)
- 3تجفيفThe combined organics were dried (MgSO4)
- 4ترشيحfiltered
- 5تركيزconcentrated in vacuo
الإجراء التجريبي
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%);