Reacción #41824

ord-0b1125e676684ac0b06b4919e8d322df

Disolventes

Condiciones de reacción

Temperatura
0°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroA clear solution resulted (pH 12), which
  2. 2
    workup.WAITat room temperature for 30 min
  3. 3
    ExtracciónThe aqueous solution was extracted with EtOAc (3×200 mL)
  4. 4
    Lavadowashed with brine (1×300 mL)
  5. 5
    Secadodried (Na2SO4)
  6. 6
    Concentraciónconcentrated

Procedimiento

To a suspension of hydroxy-[4-(4-isopropyl-piperazine-1-carbonyl) -phenyl]-methanesulfonic acid sodium salt (49.0 g, 135 mmol) in de-ionized H2O (490 mL) at 0° C. was added 1 N NaOH (100 mL) in 10 mL portions with vigorous stirring. A clear solution resulted (pH 12), which was stirred at 0° C. for 1 h, then at room temperature for 30 min. The aqueous solution was extracted with EtOAc (3×200 mL), followed by CH2Cl2 (3×200 mL). The organic layers were combined, washed with brine (1×300 mL), dried (Na2SO4) and concentrated to yield the title compound as a pale yellow oil.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07728129B2uspto-grants-2010_06