반응 #84656

ord-2b1a6636740c45f4b9d5c962b97d0fb9

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타consumption of SM
  2. 2
    workup.ADDITIONThe reaction mixture was diluted with saturated NaHCO3
  3. 3
    추출extracted with dichloromethane
  4. 4
    건조The combined organic layers were dried by Na2SO4
  5. 5
    여과filtered
  6. 6
    농축concentrated

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09434700B2uspto-grants-2016_09