Реакция #165002

ord-78e6bd01107849bd8231580d44d84968

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураunder reflux for 40 minutes
  2. 2
    Концентрированиеconcentrated under a reduced pressure
  3. 3
    ДругоеThe residue was partitioned into sodium bicarbonate solution and diethyl ether
  4. 4
    КонцентрированиеThe organic layer was concentrated under a reduced pressure
  5. 5
    Другоеthe residue was purified by silica gel chromatography (ethyl acetate)

Методика

A solution of (6-methyl-pyridin-2-yl)-methanol (1.44 g, 11.7 mmol), thionyl chloride (1.45 mL, 19.9 mmol) and methylene chloride (20 mL) was stirred under reflux for 40 minutes. The reaction solution was cooled to room temperature and then concentrated under a reduced pressure. The residue was partitioned into sodium bicarbonate solution and diethyl ether. The organic layer was concentrated under a reduced pressure, and the residue was purified by silica gel chromatography (ethyl acetate) to obtain the title compound (1.42 g, 85.8%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08841327B2uspto-grants-2014_09