Reacción #77811

ord-f6e5d696baad4eceb07ee81179ab7603

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.DISTILLATIONSolvent was distilled off under reduced pressure, and ethyl acetate
  2. 2
    workup.ADDITIONwas added to the residue, which
  3. 3
    Lavadowas washed with water and saturated brine in sequence
  4. 4
    Secadodried over anhydrous sodium sulfate
  5. 5
    workup.DISTILLATIONSolvent was distilled off under reduced pressure
  6. 6
    Otrothe residue obtained
  7. 7
    Otrowas crystallized from hexane-ethyl acetate
  8. 8
    Filtraciónthe crystals were collected by filtration

Procedimiento

To 1.00 g of 5-(2-bromo-2-carbamoylethyl)-2-methoxy-N-(4-trifluoromethylbenzyl)benzamide were added 80 ml of tetrahydrofuran and 368 mg of potassium thioacetate under an atmosphere of argon, and the mixture was stirred for 6 hours at room temperature. Solvent was distilled off under reduced pressure, and ethyl acetate was added to the residue, which was washed with water and saturated brine in sequence and dried over anhydrous sodium sulfate. Solvent was distilled off under reduced pressure, and the residue obtained was crystallized from hexane-ethyl acetate, then the crystals were collected by filtration to obtain 904 mg of 5-(2-acetylthio-2-carbamoylethyl)-2-methoxy-N-(4-trifluoromethylbenzyl)benzamide as light brown crystals.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US06706763B1uspto-grants-2004_03