تفاعل #60880

ord-36d650d9bef54b7e970ce0e95d3a1b3e

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.WAITat ambient temperature for 24 hours
  2. 2
    استخلاصThe product was extracted with EtOAc (3×15 mL)
  3. 3
    تجفيفThe combined organics were dried (MgSO4)
  4. 4
    ترشيحfiltered
  5. 5
    تركيزconcentrated 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%);

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07427616B2uspto-grants-2008_09