反応 #56844

ord-1aa52f72aeb3402696cb72c3bb6ee3a3

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過Filtration and concentration of the filtrate
  2. 2
    その他yielded a residue which
  3. 3
    その他was purified by flash chromatography on silica gel eluting with ethyl acetate-hexane (1:3)

実験手順

To a mixture of 2-amino-4,6-dichloro-5-methyl-pyrimidine (0.18 g, 1.0 mmol), 5-chloro-2-methoxy-phenyl boronic acid (0.19 g, 1.0 mmol), palladium (II) acetate (0.034 g, 0.15 mmol) and triphenylphosphine (0.079 g, 0.30 mmol) was added a solution of sodium carbonate (0.64 g, 6.0 mmol) in water (5 ml) followed by glyme (20 ml). The mixture was stirred under an argon atmosphere at room temperature for 72 hours. Filtration and concentration of the filtrate yielded a residue which was purified by flash chromatography on silica gel eluting with ethyl acetate-hexane (1:3) to provide 2-amino-4-chloro-6-(5-chloro-2-methoxyphenyl)-5-methyl-pyrimidine (0.06 g, 21% yield) as a white powder.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07419984B2uspto-grants-2008_09