Реакция #1149061

ord-d7a6da0d23cd412b8dd5363bbc21bb3f

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураcooling
  2. 2
    ДругоеA half amount of the solvent was evaporated under reduced pressure
  3. 3
    workup.ADDITIONthe residue was diluted with ethyl acetate
  4. 4
    Промывкаwashed successively with water, 1N aqueous sodium hydroxide solution, water and saturated brine
  5. 5
    Сушкаdried over magnesium sulfate
  6. 6
    ДругоеThe solvent was evaporated
  7. 7
    Промывкаthe obtained solid was washed with isopropyl ether

Методика

To a solution (800 mL) of diisopropylamine (112 mL) and triethylamine (112 mL) in THF was added dropwise a solution (400 mL) of 6-bromo-2-naphthoyl chloride in THF under ice-cooling. The mixture was stirred at room temperature for 1 hr. A half amount of the solvent was evaporated under reduced pressure, and the residue was diluted with ethyl acetate, washed successively with water, 1N aqueous sodium hydroxide solution, water and saturated brine and dried over magnesium sulfate. The solvent was evaporated and the obtained solid was washed with isopropyl ether to give the title compound (117 g) as colorless flakes.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US06960586B2uspto-grants-2005_11