Reacción #1994316

ord-a3cf34dbe8094bce807e18fb46fbdc02

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturamaintaining the temperature <30° C. with external cooling
  2. 2
    OtroThe resulting reaction mixture
  3. 3
    workup.WAITthe reaction was complete after 2 hours
  4. 4
    FiltraciónThe resulting brown suspension was filtered
  5. 5
    Lavadothe filtercake washed with cold water
  6. 6
    Otrodried in vacuo at 50° C.

Procedimiento

To a solution of 5-methyl-1,6-dihydro-pyrrolo[2,3-g]indazole-7,8-dione (23 g, 114.3 mmol) in 4N aqueous sodium hydroxide solution (160 ml) at ambient temperature, was added dropwise 30% aqueous hydrogen peroxide solution (27 ml) maintaining the temperature <30° C. with external cooling. The resulting reaction mixture was stirred at ambient temperature for 2 hours. According to TLC, the reaction was complete after 2 hours. The pH was adjusted to pH 3.5 by addition of concentrated hydrochloric acid. The resulting brown suspension was filtered and the filtercake washed with cold water and dried in vacuo at 50° C. to afford the desired product as brown solid. LC/MS: 192 (M+H)+.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08598078B2uspto-grants-2013_12