Reacción #64705

ord-336b3b8c2eb143d68f7aa0398be0a69a

Disolventes

Condiciones de reacción

Temperatura
60°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.ADDITIONwere added
  2. 2
    workup.STIRRINGThe stirring of the resulting mixture
  3. 3
    workup.WAITwas continued for 1 hour
  4. 4
    Extracciónextracted with methylene chloride
  5. 5
    LavadoThe organic layer was washed with saturated brine
  6. 6
    Secadodried over anhydrous magnesium sulfate
  7. 7
    OtroThe solvent was evaporated under reduced pressure
  8. 8
    Lavadoeluted with hexane-ethyl acetate (5:1)

Procedimiento

A mixture of 2-methylbenzoyl chloride (1.55 g) and methyl isocyanide (492 mg) was stirred at 60° C. for 6 hours. Then, the mixture was diluted with acetone (20 ml), and water (4 ml) and calcium carbonate (1.00 g) were added. The stirring of the resulting mixture was continued for 1 hour. The mixture was neutralized with dilute hydrochloric acid and extracted with methylene chloride. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was subjected to column chromatography on silica gel and eluted with hexane-ethyl acetate (5:1) to obtain the title compound (1.71 g, Yield: 96.6%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05414122uspto-grants-1995_05