Reacción #2828

ord-afe1acea3c9c4770b2b372a33f6672d6

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturawhile cooling on ice
  2. 2
    ExtracciónThe whole was extracted with ethyl acetate
  3. 3
    Lavadowashed with 5% sodium hydrogencarbonate aqueous solution and water
  4. 4
    Secadodried over anhydrous sodium sulfate
  5. 5
    OtroThe solvent was evaporated
  6. 6
    Otrothe residue was purified by silica gel column chromatography (Kieselgel 60=170 g, hexane/ethyl acetate=3/1)
  7. 7
    Otroto obtain the above-captioned compound ([6]-(62)-90) (7.70 g) as a white solid

Procedimiento

To anhydrous pyridine (120 ml), methyl 3-aminobenzoate (5.00 g) was dissolved, and valeryl chloride (4.13 ml) was added while cooling on ice. The mixture was stirred at room temperature for 4 hours. Distilled water was added to the solution. The whole was extracted with ethyl acetate, washed with 5% sodium hydrogencarbonate aqueous solution and water, and dried over anhydrous sodium sulfate. The solvent was evaporated, and the residue was purified by silica gel column chromatography (Kieselgel 60=170 g, hexane/ethyl acetate=3/1) to obtain the above-captioned compound ([6]-(62)-90) (7.70 g) as a white solid.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05731310uspto-grants-1998_03