Реакция #216841

ord-9155643392d24aaf93d4caf7a876ff5e

Условия реакции

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

Обработка

  1. 1
    ТемператураThe solution is cooled to a temperature in the region of 20° C.
  2. 2
    ЭкстракцияAcidification is carried out to a pH in the region of 2 using 4N hydrochloric acid and extraction
  3. 3
    ПромывкаThe organic phase is washed with a total of 450 cm3 of distilled water
  4. 4
    Сушкаdried over magnesium sulphate
  5. 5
    Концентрированиеconcentrated under reduced pressure (13.5 Pa) at a temperature in the region of 60° C

Методика

12.3 g of methyl 11-bromo-2,2-dimethylundecanoate in solution in 70 cm3 of N,N-dimethylformamide are added to 8.2 g of potassium phthalimide in 70 cm3 of N,N-dimethylformamide and the mixture is heated for 3 hours at a temperature in the region of 80° C. The solution is cooled to a temperature in the region of 20° C. and then poured into 1400 cm3 of distilled water. Acidification is carried out to a pH in the region of 2 using 4N hydrochloric acid and extraction is then carried out with a total of 1000 cm3 of ethyl acetate. The organic phase is washed with a total of 450 cm3 of distilled water, dried over magnesium sulphate, and then concentrated under reduced pressure (13.5 Pa) at a temperature in the region of 60° C. 15.4 g of methyl 11-phthalimido-2,2-dimethylundecanoate are thus obtained in the form of a pale yellow viscous oil [Rf =0.38; silica thin layer chromatography; eluent: cyclohexane/ethyl acetate 8/2 (by volume)].

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05468888uspto-grants-1995_11