Реакция #8538

ord-8b10cb0936e1470cb7743fcc2219590f

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеat 0° C
  2. 2
    Другоеthe solvent was evaporated
  3. 3
    workup.ADDITIONAfter adding water
  4. 4
    Промывкаthe residue was washed with chloroform
  5. 5
    workup.ADDITIONNext, hydrochloric acid (6 mol/l) was slowly added to the aqueous layer until pH value
  6. 6
    ЭкстракцияThen the aqueous layer was extracted with diisopropyl ether (IPE)
  7. 7
    СушкаThe organic layer was dried over anhydrous magnesium sulfate
  8. 8
    Другоеthe solvent was evaporated

Методика

Methyl 2-(2,3,4-trifluoroanilino)propionate (46.64 g) was dissolved in methanol (130 ml) and an aqueous solution (3 mol/l; 100 ml) of lithium hydroxide was slowly added thereto at 0° C. After stirring at room temperature for 3 hours, the solvent was evaporated. After adding water, the residue was washed with chloroform. Next, hydrochloric acid (6 mol/l) was slowly added to the aqueous layer until pH value reached 1. Then the aqueous layer was extracted with diisopropyl ether (IPE). The organic layer was dried over anhydrous magnesium sulfate and then the solvent was evaporated to give the title compound (43.7 g) as colorless crystals.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07087778B2uspto-grants-2006_08