Реакция #75357

ord-0070be7f38a14afa8e5cf102433dffa7

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеthe temperature below 30° C
  2. 2
    Другоеto rise to 30° C
  3. 3
    Экстракцияthe subsequent mixture was extracted with ether
  4. 4
    ПромывкаThe combined extracts were washed with water
  5. 5
    Сушкаdried (MgSO4)
  6. 6
    Другоеevaporated

Методика

Sodium hydride (0.45 g., 80% w/w suspension in mineral oil) was added gradually to a stirred solution of 4,4'-dichlorobenzophenone oxime (4.0 g.) in dry dimethylformamide (20 ml.) keeping the temperature below 30° C. After 30 minutes, ethyl bromoacetate (1.7 ml.) was added to the stirred solution and the temperature was allowed to rise to 30° C. After 16 hours stirring at ambient temperature the mixture was poured into water (100 ml.) and the subsequent mixture was extracted with ether. The combined extracts were washed with water, dried (MgSO4) and evaporated to give ethyl di-(4-chlorophenyl)methyleneamino-oxyacetate, as an oil (3.8 g.), essentially pure and having a characteristic ester absorption at 1740-1760 cm-1 in the infra-red spectrum.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04176194uspto-grants-1979_11