Reacción #80291

ord-172b663c480f428491802387607eff65

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    FiltraciónThe solid was filtered off
  2. 2
    Concentraciónresidue was concentrated under reduced pressure
  3. 3
    Extracciónextracted with ethyl acetate
  4. 4
    LavadoThe organic layer was washed with water
  5. 5
    Secadodried over anhydrous sodium sulfate
  6. 6
    OtroThe residue obtained by concentration under reduced pressure
  7. 7
    Otrowas crystallized from isopropyl ether

Procedimiento

3.4 g of allyl 5-[(4,6-dimethoxypyrimidin-2-yl)oxy]-2-methyl-3-nitroindol-4-carboxylate was dissolved in 50 ml of methanol, and 5 ml of concentrated hydrochloric acid was added thereto. Then, 4.9 g of tin powder was gradually added at room temperature. Them, the mixture was stirred at room temperature for 12 hours. The solid was filtered off, and then residue was concentrated under reduced pressure and extracted with ethyl acetate. The organic layer was washed with water and then dried over anhydrous sodium sulfate. The residue obtained by concentration under reduced pressure, was crystallized from isopropyl ether to obtain 2.5 g (yield: 79%) of the desired product. mp: 132°-135° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05616537uspto-grants-1997_04