Reacción #455475

ord-a77702c573d44e00a5c2f1f77cf14353

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otrowas bubbled through the reaction mixture
  2. 2
    Filtraciónfiltered
  3. 3
    Otrothe filtrate evaporated to dryness under reduced pressure
  4. 4
    OtroRecrystallisation of the residue from hexane

Procedimiento

5,6-Dichloro-N-hydroxy-3-pyridinecarboximidoyl chloride (0.85 g, 3.8 mmol) was dissolved with stirring in ether (60 mL) and a solution of triethylamine (0.8 g, 7.9 mmol) in ether (50 mL) added dropwise to the solution while 1-butyne was bubbled through the reaction mixture. The mixture was stirred at room temperature overnight, filtered, and the filtrate evaporated to dryness under reduced pressure. Recrystallisation of the residue from hexane gave the desired product (0.83 g, 90%) as a cream solid, melting point. 98-9° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US06133294uspto-grants-2000_10