Reacción #88660

ord-6db0c35485e640179f32a44cfd03d72d

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    FiltraciónThe resulting precipitate was collected by filtration
  2. 2
    Lavadowashed with diethyl ether

Procedimiento

To a solution of N-(1-(1-cyclopropyl-1-oxopropan-2-yl)-5-iodopyridin-2(1H)-ylidene)-4-methylbenzenesulfonamide (30.5 g) in THF (300 mL) was added trifluoroacetic anhydride (18.3 mL) dropwise, and the mixture was stirred for 3 hr. The resulting precipitate was collected by filtration, and washed with diethyl ether to give a salt of the title compound as a white solid. The obtained solid was dissolved in 1 N sodium hydroxide, and the solution was extracted with ethyl acetate/THF. Then the organic layer was washed with brine, dried over sodium sulfate and concentrated in vacuo. The obtained solid was washed with diisopropyl ether to give the title compound (17.7 g) as a yellow solid.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US09440987B2uspto-grants-2016_09