Reacción #93486

ord-cfbb51c4de9446b3ae8f6ac9ea57ff96

Disolventes

Condiciones de reacción

Temperatura
90°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Extracciónthe mixture was extracted with ethyl acetate
  2. 2
    LavadoThe extract was washed with water saturated with sodium chloride
  3. 3
    Secadodried over anhydrous sodium sulfate
  4. 4
    Concentraciónconcentrated
  5. 5
    workup.DISSOLUTIONThe thus produced residue was dissolved in acetone
  6. 6
    workup.ADDITIONconcentrated hydrochloric acid in an amount of 2 equivalents was added
  7. 7
    Otroto produce crystals
  8. 8
    FiltraciónThe crystals were filtered off

Procedimiento

A mixture of 2 g of 5-(5-chlorovaleryl)-2-benzyloxy-benzamide, 1 g of 1-phenylpiperazine, 0.6 g of sodium carbonate and 10 ml of dimethyl sulfoxide was heated at 90° C. for 6 hours while stirring. After the reaction was finished, water was added to the reaction mixture and the mixture was extracted with ethyl acetate. The extract was washed with water saturated with sodium chloride, dried over anhydrous sodium sulfate and concentrated. The thus produced residue was dissolved in acetone and concentrated hydrochloric acid in an amount of 2 equivalents was added thereto to produce crystals. The crystals were filtered off to obtain 2.3 g of 5-[5-(4-phenyl-1-piperazinyl)valeryl]-2-benzyloxy-benzamide (yield: 73%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04613598uspto-grants-1986_09