Реакция #42015

ord-bd280309d1274ad4b0b18844835c296f

Реагенты

Растворители

Условия реакции

Температура
80°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONwas added
  2. 2
    Фильтрацияthe catalyst was filtered off
  3. 3
    ДругоеThe organic layer was separated
  4. 4
    Экстракцияthe aqueous phase was extracted with ether (2×50 ml)
  5. 5
    ПромывкаThe combined organic extracts were washed with water (25 ml)
  6. 6
    Сушкаdried with anhydrous magnesium sulphate
  7. 7
    Концентрированиеconcentrated

Методика

A mixture of Ceiv catalyst from Example 47 (0.08 g), sodium bromate (0.3 g) and benzyl alcohol (0.216 g, 2 mmol) in acetonitrile:water (5:7, 12 ml) was stirred at 80° C. for 40 h under an atmosphere of nitrogen. On cooling ether (70 ml) was added and the catalyst was filtered off. The organic layer was separated and the aqueous phase was extracted with ether (2×50 ml). The combined organic extracts were washed with water (25 ml), dried with anhydrous magnesium sulphate and concentrated to give benzoic acid as a white solid (0.22 g, 90%). M.p. 120° C., lit. 120-122° C.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07728159B2uspto-grants-2010_06