Reaktion #937127

ord-0e58a827d880489793b8875111bf1337

Reaktionsbedingungen

Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter completion of the reaction
  2. 2
    workup.WAITthe reaction mixture was left
  3. 3
    Temperaturcooling to room temperature
  4. 4
    workup.DISTILLATIONthe excess ethyl chloroformate was distilled out under reduced pressure
  5. 5
    SonstigeThe residue was recrystallized from hexane, which

Vorschrift

A mixture of 0.35 g of 3-(5-amino-2,4-dichlorophenyl)-1-methyl-6-trifluoromethyl-2-oxo-1,2-dihydropyrazine (present compound 1-334) and 3.1 ml of ethyl chloroformate was stirred at 100° C. for 2 hours. After completion of the reaction, the reaction mixture was left cooling to room temperature, and the excess ethyl chloroformate was distilled out under reduced pressure. The residue was recrystallized from hexane, which afforded 0.32 g (yield, 79%) of 3-(2,4-dichloro-5-ethoxycarbonylaminophenyl)-1-methyl-6-trifluoromethyl-2-oxo-1,2-dihydropyrazine (present compound 1-346; m.p., 116.2-C).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06015774uspto-grants-2000_01