반응 #87435

ord-f0147134e4364c48bd4999c5edf3e11c

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타was quenched with ammonium chloride (aq, sat)
  2. 2
    기타The solvent volume was reduced by evaporation
  3. 3
    추출The mixture was extracted with dichloromethane
  4. 4
    농축concentrated in vacuum
  5. 5
    기타The residue was purified by preparative HPLC

실험 절차

To an ice-cold solution of cyclopropylmagnesium bromide (1.90 mL, 0.95 mmol) in THF (10 mL), a solution of 2-(3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenylamino)-6-((2,2,2-trifluoroethoxy)methyl)pyrimidine-4-carbaldehyde (40 mg, 0.09 mmol) in THF (6 mL) was added over 5 min. The mixture was stirred on ice-bath for 30 minutes before it was quenched with ammonium chloride (aq, sat). The solvent volume was reduced by evaporation. The mixture was extracted with dichloromethane, the organic phase was passed through a phase separator and concentrated in vacuum. The residue was purified by preparative HPLC to give the title compound as a dry film, 7 mg (16%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09439904B2uspto-grants-2016_09