Реакция #2056344

ord-25dbc57c3db940b188553842ba0102e8

Реагенты

Нет

Условия реакции

Температура
60°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураthe mixture is cooled to room temperature
  2. 2
    Другоеn-Hexylamine is removed under reduced pressure
  3. 3
    workup.DISSOLUTIONThe residue is dissolved in ethyl acetate
  4. 4
    Экстракцияfurther extracted with 1 N HCl
  5. 5
    ЭкстракцияThe organic layer is extracted with saturated sodium bicarbonate
  6. 6
    Сушкаdried over anhydrous sodium sulfate
  7. 7
    ДругоеSolvent is removed under reduced pressure

Методика

Methyl 2,5-dihydroxybenzoate (1 g) is dissolved in 10 mL of n-hexylamine. After overnight heating in an oil bath (60° C.), the mixture is cooled to room temperature. n-Hexylamine is removed under reduced pressure. The residue is dissolved in ethyl acetate and further extracted with 1 N HCl. The organic layer is extracted with saturated sodium bicarbonate and dried over anhydrous sodium sulfate. Solvent is removed under reduced pressure to yield the product as an off-white powder.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08426466B2uspto-grants-2013_04