반응 #60880

ord-36d650d9bef54b7e970ce0e95d3a1b3e

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.WAITat ambient temperature for 24 hours
  2. 2
    추출The product was extracted with EtOAc (3×15 mL)
  3. 3
    건조The combined organics were dried (MgSO4)
  4. 4
    여과filtered
  5. 5
    농축concentrated in vacuo

실험 절차

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%);

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07427616B2uspto-grants-2008_09