Reacción #1697282

ord-a9838a8399f34b5f8aa72dd636381270

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.STIRRINGby stirring at room temperature for 1 hour
  2. 2
    LavadoThe organic layer was sequentially washed with saturated aqueous ammonium chloride solution and brine
  3. 3
    Secadodried over anhydrous magnesium sulfate
  4. 4
    Otrothe solvent was evaporated
  5. 5
    LavadoThe resulting crude crystals were washed with diethyl ether

Procedimiento

To a solution of 27.5 g of 3-iodo-5-nitro-1H-indazole in 300 ml tetrahydrofuran at 0° C. in an atmosphere of nitrogen gas was added 6.1 g of 60% sodium hydride, and the mixture was stirred at the same temperature for 10 minutes. To the mixture was added 39.8 g of trityl chloride, followed by stirring at room temperature for 1 hour. Water was added and the mixture was diluted with ethyl acetate. The organic layer was sequentially washed with saturated aqueous ammonium chloride solution and brine, dried over anhydrous magnesium sulfate and the solvent was evaporated. The resulting crude crystals were washed with diethyl ether, to give 48.5 g of the title compound as colorless crystals.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US06982274B2uspto-grants-2006_01