Реакция #675973

ord-0317cada9178428eb4100ae6dbf068a7

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    КонцентрированиеThe mixture was concentrated in vacuo
  2. 2
    Другоеthe residue was purified by flash column chromatography on silica gel (petroleum ether/ethyl acetate=20:1 to 5:1)

Методика

A mixture of 2-(2-(4,5-dichloro-2-iodophenoxy)pyridin-4-yloxy)ethanol (130 mg, 0.31 mmol), isoindoline-1,3-dione (54 mg, 0.37 mmol), PPh3 (160 mg, 0.61 mmol) in THF (5 mL) at 0° C., DIAD (123 mg, 0.61 mmol) was added. The resulting mixture was allowed to warm to room temperature and stirred for 15 h. The mixture was concentrated in vacuo and the residue was purified by flash column chromatography on silica gel (petroleum ether/ethyl acetate=20:1 to 5:1) to afford the desired product (120 mg, 71% yield). ESI-MS m/z: 555.0[M+H]+.

Источник

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