반응 #330367

ord-97e3b0a0e1b14419b3bb23f6c34ccc5b

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축The reaction mixture was concentrated in vacuo
  2. 2
    기타the residue purified by chromatography
  3. 3
    세척eluting with (SiO2 0-80% DCM in cyclohexane)

실험 절차

Methylamine (2M in THF, 19 mL, 38.1 mmol) was added to a solution of 2-bromo-1,3-difluoro-4-nitrobenzene (4.53 g, 19 mmol) and DIPEA (6.8 mL, 38.1 mmol) in THF (70 mL) and the resultant mixture stirred at 60° C. for 3 h. The reaction mixture was concentrated in vacuo and the residue purified by chromatography eluting with (SiO2 0-80% DCM in cyclohexane) to give title compound as an orange/yellow solid (4.32 g, 91%). LCMS (Method C): RT 3.46 min [M+H]+ 249.0, 251.0.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08653089B2uspto-grants-2014_02