Reacción #66811

ord-cd6a9ede643640a1a846cbef67ddd10c

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    ConcentraciónThe mixture was then concentrated in vacuo
  2. 2
    Otrothe residue was triturated with petroleum ether
  3. 3
    Otrothe solvent was decanted
  4. 4
    OtroThe remaining solid was then triturated with diethyl ether/petroleum ether (1:1)
  5. 5
    Filtraciónthe precipitate was collected by suction filtration

Procedimiento

Ethyl 2-amino-3-cyano-4,7-dihydrofuro[2,3-c]pyridine-6(5H)-carboxylate from Example 36A (7.00 g, 29.8 mmol) was heated in dimethylformamide dimethylacetal (14.7 mL, 110 mmol) for 30 min to 110° C. The mixture was then concentrated in vacuo, and the residue was triturated with petroleum ether, the solvent was decanted, and the trituration was repeated. The remaining solid was then triturated with diethyl ether/petroleum ether (1:1), and the precipitate was collected by suction filtration to yield 8.5 g (98%) of the title compound.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08524722B2uspto-grants-2013_09