Reacción #67143

ord-41128cd80b9f4d918ca1c43edf31c1e4

Condiciones de reacción

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

Tratamiento posterior

  1. 1
    TemperaturaThe reaction was heated in the microwave for a further 20 mins
  2. 2
    OtroThe (2R,6S)-2,6-dimethylmorpholine was removed
  3. 3
    OtroThe solvent was removed
  4. 4
    Otrothe residue purified by Mass Directed Automated Preparative HPLC (Method B)
  5. 5
    OtroThe desired product was not collected so the waste
  6. 6
    Concentraciónwas concentrated in vacuo
  7. 7
    Otrothe residue purified by Mass Directed Automated Preparative HPLC (Method B)

Procedimiento

N-(2-Chloro-5-{4-[5-(chloromethyl)-1,3,4-oxadiazol-2-yl]-1-[(4-methylphenyl)sulfonyl]-1H-indazol-6-yl}-3-pyridinyl)methanesulfonamide (50 mg, 0.084 mmol) and (2R,6S)-2,6-dimethylmorpholine (0.5 ml, 0.084 mmol) were placed a vial and heated in a microwave at 90° C. for 15 mins. The reaction was heated in the microwave for a further 20 mins. The (2R,6S)-2,6-dimethylmorpholine was removed and the residue placed into isopropanol (3 ml) and 2M sodium hydroxide (1 ml) and the mixture stirred at room temperature for 3 h. The solvent was removed and the residue purified by Mass Directed Automated Preparative HPLC (Method B). The desired product was not collected so the waste was concentrated in vacuo and the residue purified by Mass Directed Automated Preparative HPLC (Method B) to give the title compound as white solid (12 mg).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08524751B2uspto-grants-2013_09