Reacción #77920

ord-1f4befc33ffa492db518647e07a976d7

Disolventes

Condiciones de reacción

Temperatura
220°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.ADDITIONwas added to a reactor
  2. 2
    TemperaturaThe reaction mixture was cooled down to room temperature
  3. 3
    OtroToluene layer separated
  4. 4
    Secadowas dried over anhydrous MgSO4
  5. 5
    Filtraciónfiltered
  6. 6
    Otroevaporated
  7. 7
    Otroto give crude product
  8. 8
    OtroThe crude product was purified by column chromatograph on silica gel
  9. 9
    Lavadoby eluting with a mixture of ethylacetate and n-hexane (1:5)

Procedimiento

A mixture of 7-(2-naphthoyl)-3-methyl-5,6-dihydro-2(4H)-benzofuranone (10 g) and acetic acid potassium salt (0.3 g) was added to a reactor and stirred for 1 hr at 220° C. The reaction mixture was cooled down to room temperature. Toluene and water were added to the reaction mixture and acidified to pH 2 with 5% hydrochloric acid. Toluene layer separated was dried over anhydrous MgSO4, filtered and evaporated to give crude product. The crude product was purified by column chromatograph on silica gel by eluting with a mixture of ethylacetate and n-hexane (1:5) to give the desired product (9:42 g, 94 % .

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US06706917B1uspto-grants-2004_03