Reacción #84656

ord-2b1a6636740c45f4b9d5c962b97d0fb9

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otroconsumption of SM
  2. 2
    workup.ADDITIONThe reaction mixture was diluted with saturated NaHCO3
  3. 3
    Extracciónextracted with dichloromethane
  4. 4
    SecadoThe combined organic layers were dried by Na2SO4
  5. 5
    Filtraciónfiltered
  6. 6
    Concentraciónconcentrated

Procedimiento

A mixture of tert-butyl ((1S,2R)-2-((6-(2,6-dichloro-3,5-dimethoxyphenyl)quinazolin-2-yl)amino)cyclohexyl)carbamate (67 mg, 0.12 mmol) and TFA (0.6 mL) in dichloromethane (0.6 mL) was stirred at room temperature for 60 minutes. LC-MS indicated complete consumption of SM. The reaction mixture was diluted with saturated NaHCO3 and then extracted with dichloromethane. The combined organic layers were dried by Na2SO4, filtered, concentrated to give (1R,2S)—N1-(6-(2,6-dichloro-3,5-dimethoxyphenyl)quinazolin-2-yl)cyclohexane-1,2-diamine which was used without further purification in the next step.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US09434700B2uspto-grants-2016_09