Реакция #1249

Уравнение реакции

product

Ethyl 2,4-dioxo-4-(2,4,6-trimethylphenyl)butanoate

HCl

NaNO2

→

semi-solid

Ethyl 2,4-dioxo-3-oximino-4-(2,4,6-trimethylphenyl)butanoate

Растворители

ethanol

Условия реакции

Обработка

1. 1
   ДругоеThe solvent was removed from the mixture and 200 mL of water
2. 2
   workup.ADDITIONwas added to the residue
3. 3
   ЭкстракцияThe product was then extracted into ether
4. 4
   ЭкстракцияThe ether extract
5. 5
   Сушкаwas dried over Na2SO4
6. 6
   Другоеevaporated

Методика

N2O3 gas was slowly passed into a stirred solution of the product of step A (16.2 g) in 300 mL of ethanol until the disappearance of starting material was confirmed by TLC. N2O3 gas was generated by the dropwise addition of 12N aqueous HCl solution into an aqueous slurry of NaNO2. The solvent was removed from the mixture and 200 mL of water was added to the residue. The product was then extracted into ether. The ether extract was dried over Na2SO4 and evaporated to give 16.1 g of a semi-solid.

Источник