Реакция #64071

ord-1c896af0227b495fb2c8ee6f51728118

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONInto a beaker, are added
  2. 2
    workup.STIRRINGThe reaction medium is stirred
  3. 3
    Температураcooled to between 5° and 10° C
  4. 4
    workup.STIRRINGThe mixture is stirred for 30 min at room temperature
  5. 5
    Фильтрацияthe clear mixture is filtered
  6. 6
    ДругоеThe filtrate is evaporated to dryness
  7. 7
    ДругоеAn oil is obtained which
  8. 8
    Другоеcrystallizes at room temperature
  9. 9
    ФильтрацияIt is filtered on sintered glass
  10. 10
    ДругоеThe white powder obtained
  11. 11
    Сушкаis dried under vacuum over phosphoric anhydride

Методика

Into a beaker, are added, with stirring, 11.4 g (0.06 mole) of triisopropanolamine in 100 ml of isopropanol. The reaction medium is stirred and cooled to between 5° and 10° C. 19.2 g (0.06 mole) of 5-n-dodecanoylsalicylic acid are then added. The mixture is stirred for 30 min at room temperature and then the clear mixture is filtered. The filtrate is evaporated to dryness. An oil is obtained which crystallizes at room temperature. It is filtered on sintered glass. The white powder obtained is dried under vacuum over phosphoric anhydride. 29.1 g of product are obtained, equivalent to a yield of 95%.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05411742uspto-grants-1995_05