Reacción #164955

ord-98b3f4f817b84beb8c6d3ab9195fe6f3

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.ADDITIONThe reaction mixture were poured into ice-cold aqueous Na2CO3 solution
  2. 2
    Extracciónextracted with ethyl acetate
  3. 3
    LavadoThe organic layer washed with brine
  4. 4
    Secadodried over anhydrous Na2SO4
  5. 5
    Filtraciónfiltered
  6. 6
    Concentraciónconcentrated in vacuo

Procedimiento

A mixture of NaN3 (481 mg, 7.4 mmol) and 5-[1-chloro-2,2,2-trifluoro-eth-(Z)-ylideneamino]-4′-methyl-biphenyl-3-carboxylic acid methyl ester (1.3 g, 3.7 mmol) in 10 ml of dry ACN was stirred at room temperature for 16 hours. The reaction mixture were poured into ice-cold aqueous Na2CO3 solution, extracted with ethyl acetate. The organic layer washed with brine, dried over anhydrous Na2SO4, filtered, and concentrated in vacuo. The resulting crude 4′-methyl-5-(5-trifluoromethyl-tetrazol-1-yl)-biphenyl-3-carboxylic acid methyl ester (1.34 g, 99% yield) was used directly in the next step.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08841336B2uspto-grants-2014_09