Reaktion #446287

ord-74b4bcc07ef34a868f69532ad9f05354

Reaktionsgleichung

CCOC(=O)C(CC)C(=O)OCC
Diethyl 2-ethylmalonate
Nc1ccc(Cl)cc1
p-chloroaniline
CCOC(=O)C(CC)C(=O)Nc1ccc(Cl)cc1
desired product
CCOC(=O)C(CC)C(=O)Nc1ccc(Cl)cc1
Ethyl 2-(4-chlorophenylcarbamoyl)butyrate

Lösungsmittel

Reaktionsbedingungen

Temperatur
130°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe mixture was cooled
  2. 2
    Waschenfurther, the mixture was washed successively with 1N hydrochloric acid, aqueous sodium bicarbonate solution, and water
  3. 3
    Einengenconcentrated under reduced pressure
  4. 4
    Wascheneluted with chloroform

Vorschrift

Diethyl 2-ethylmalonate (8.76 ml) and p-chloroaniline (4 g) were dissolved by heating at 130° C. for 11 hours, and the mixture was cooled and dissolved in ethyl acetate, and further, the mixture was washed successively with 1N hydrochloric acid, aqueous sodium bicarbonate solution, and water, and concentrated under reduced pressure. The resulting residue was subjected to column chromatography on silica gel and eluted with chloroform to give the oily desired product (6.66 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04999378uspto-grants-1991_03