Реакция #463611

ord-8478ae9ce00f4aafb8ce937a724cad71

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураat reflux 1.5 h
  2. 2
    ДругоеPartitioned between ethyl acetate (150 mL) and saturated sodium bicarbonate(150 mL)
  3. 3
    ДругоеOrganic phase was separated
  4. 4
    Промывкаwashed with water (5×75 mL), brine (75 mL)
  5. 5
    Сушкаdried over sodium sulfate (anhy.)
  6. 6
    Фильтрацияfiltered
  7. 7
    Концентрированиеconcentrated

Методика

To a solution of 2-fluoro-5-nitrobenzonitrile (2.0 g, 12 mmol) in ethyl acetate(50 mL) was added stannous chloride (27.0 g, 120 mmol). The reaction mixture was stirred at reflux 1.5 h, then cooled to room temperature. Partitioned between ethyl acetate (150 mL) and saturated sodium bicarbonate(150 mL). Organic phase was separated and washed with water (5×75 mL), brine (75 mL); dried over sodium sulfate (anhy.); filtered and concentrated to give 2-fluoro-5-aminobenzonitrile (1.4 g) as pure compound.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US06020357uspto-grants-2000_02