Реакция #84418

ord-edd3c005b7ff421e8b4b6e91a40db2c3

Реагенты

Нет

Растворители

Условия реакции

Температура
90°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураcooled to rt
  2. 2
    Экстракцияextracted with CH2Cl2 (80 mL×3)
  3. 3
    СушкаThe combined organic phases were dried over anhydrous Na2SO4
  4. 4
    Концентрированиеconcentrated in vacuo
  5. 5
    ДругоеThe residue was purified by a silica gel column chromatography (PE/CH2Cl2 (V/V)=10:1)

Методика

To a solution of 3,4-difluoronitrobenzene (3.18 g, 20 mmol) in DMSO (25 mL) were added K2CO3 (6.08 g, 44 mmol) and di-n-butylamine (2.84 g, 22 mmol) with stirring. The mixture was heated at 90° C. overnight, then cooled to rt, diluted with water (100 mL) and extracted with CH2Cl2 (80 mL×3). The combined organic phases were dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/CH2Cl2 (V/V)=10:1) to give the title compound as yellow oil (4.03 g, 75%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09434695B2uspto-grants-2016_09