Реакция #70285

ord-18d6551235cd4ddda8d73eb9a4e6944b

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONwas added slowly until pH=4-5
  2. 2
    ДругоеThe suspension obtained
  3. 3
    Фильтрацияwas filtered
  4. 4
    Другоеthe filtrate evaporated
  5. 5
    ДругоеThe solid obtained
  6. 6
    Промывкаwashed with water and brine
  7. 7
    Другоеdried
  8. 8
    Концентрированиеconcentrated

Методика

To a solution of 5-bromo-2-(2,6-difluoro-4-methoxyphenyl)pyrimidine (0.887 g, 2.95 mmol) in DCM at 0° C., was added dropwise a solution of BBr3 (1M in DCM) (22 ml, 22 mmol) and the reaction mixture was stirred overnight at room temperature. This mixture was then poured over cold MeOH and solid NaHCO3 was added slowly until pH=4-5. The suspension obtained was filtered and the filtrate evaporated. The solid obtained was redissolved in ethyl acetate, washed with water and brine, dried and concentrated to give the desired compound as a white solid (0.817 g, 85% of yield).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08536165B2uspto-grants-2013_09