Реакция #50912

ord-82b51a0afe8b45b9b3dbcd705924a1bb

Реагенты

Нет

Растворители

Условия реакции

Температура
5°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ФильтрацияThe white solid was filtered
  2. 2
    ДругоеThe filtercake was air-dried
  3. 3
    Другоеrecrystallized from ethyl acetate/heptane

Методика

A solution of 2-chloro-4-fluorobenzoic acid (24.4 g, 0.142 mol) in 150 ml of concentrated sulfuric acid at 0° C. was treated dropwise with 90% nitric acid (13.2 ml, 20 mol %, 0.284 mol) over a 10 min. period at 10° C., stirred for 2.5 hours at 0 to 10° C., poured onto one liter of ice. The white solid was filtered. The filtercake was air-dried and recrystallized from ethyl acetate/heptane to afford the title compound as off-white needles. Yield: 18.0 g (58.1%); identified by NMR spectral analysis.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US06849618B2uspto-grants-2005_02