Реакция #75358

Уравнение реакции

ethyl di-(4-chlorophenyl)methyleneamino-oxyacetate

sodium hydroxide

→

di-(4-chlorophenyl)methyleneamino-oxyacetic acid

Выход 33.0%

Растворители

ethanol

water

Условия реакции

Обработка

1. 1
   Температураwas heated
2. 2
   Температураunder reflux for 16 hours
3. 3
   ДругоеThe mixture was then evaporated
4. 4
   workup.ADDITIONthe residue was diluted with water (100 ml.) and ether (50 ml.)
5. 5
   ДругоеThe ether layer was separated
6. 6
   workup.ADDITIONThe aqueous layer was acidified to pH 2-3 by addition of 20% v/v hydrochloric acid
7. 7
   Другоеthe solid (3.0 g.) which formed
8. 8
   Другоеwas separated
9. 9
   Другоеcrystallised from ethyl acetate

Методика

A solution of ethyl di-(4-chlorophenyl)methyleneamino-oxyacetate (3.8 g.) in ethanol (140 ml.) and water (5 ml.) containing sodium hydroxide (5 g.) was heated under reflux for 16 hours. The mixture was then evaporated and the residue was diluted with water (100 ml.) and ether (50 ml.). The ether layer was separated and discarded. The aqueous layer was acidified to pH 2-3 by addition of 20% v/v hydrochloric acid and the solid (3.0 g.) which formed was separated and crystallised from ethyl acetate to give di-(4-chlorophenyl)methyleneamino-oxyacetic acid, m.p. 147°-148° C., in 33% yield.

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