Реакция #60880

ord-36d650d9bef54b7e970ce0e95d3a1b3e

Условия реакции

Температура
0°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.WAITat ambient temperature for 24 hours
  2. 2
    ЭкстракцияThe product was extracted with EtOAc (3×15 mL)
  3. 3
    СушкаThe combined organics were dried (MgSO4)
  4. 4
    Фильтрацияfiltered
  5. 5
    Концентрированиеconcentrated in vacuo

Методика

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%);

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07427616B2uspto-grants-2008_09