Реакция #675974

ord-926d235f12224ea9932dc121dca52f8c

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураat reflux for 1 h
  2. 2
    Концентрированиеconcentrated in vacuo
  3. 3
    ДругоеThe precipitate was removed by filtration
  4. 4
    Концентрированиеthe filtrate was concentrated in vacuo
  5. 5
    ДругоеThe residue was purified by flash column chromatography on silica gel (DCM/MeOH=10:1)

Методика

The mixture of 2-(2-(2-(4,5-dichloro-2-iodophenoxy)pyridin-4-yloxy)ethyl)isoindoline-1,3-dione (120 mg, 0.22 mmol), N2H4.H2O (106 mg, 1.80 mmol) and EtOH (5 mL) was stirred at reflux for 1 h. The mixture was allowed to cool to room temperature and then concentrated in vacuo. The residue was slurried in DCM (5 mL) and MeOH (1 mL). The precipitate was removed by filtration, and the filtrate was concentrated in vacuo. The residue was purified by flash column chromatography on silica gel (DCM/MeOH=10:1) to afford the desired product (35 mg, 38% yield).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09227978B2uspto-grants-2016_01