반응 #329872

ord-b57d5ff52afe4dbbae5895aac90f5ebb

용매

반응 조건

온도
110°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The solvent was evaporated
  2. 2
    세척washed with saturated aqueous sodium bicarbonate and brine
  3. 3
    건조dried over magnesium sulfate

실험 절차

To a mixture of 4-chlorobromobenzene (0.53 g, 2.75 mmol) and 3-(R)-Methyl-piperazine-1-carboxylic acid tert-butyl ester (0.5 g, 2.5 mmol) in toluene (20 mL) was added tris(dibenzylideneacetone) dipalladium(0) (0.029 g, 0.032 mmol), BINAP (0.058 g, 0.093 mmol) and sodium-t-butoxide (1.01 g, 10.5 mmol). The resulting mixture was heated 110° C. for 20 h. The solvent was evaporated and the residue was taken up in ethyl acetate and washed with saturated aqueous sodium bicarbonate and brine and dried over magnesium sulfate. Column chromatography (10% ethyl acetate/hexane) provided the title compound.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08653096B2uspto-grants-2014_02