反応 #70047

ord-54e93a156bda4084bf6d52b0eed88b98

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The compound was synthesized
  2. 2
    その他The volatiles were evaporated
  3. 3
    その他the residue was partitioned between sodium bicarbonate solution and MeOH/CHCl3 (5/95)
  4. 4
    洗浄The organic layer was washed with brine
  5. 5
    乾燥dried over Na2SO4
  6. 6
    その他evaporated
  7. 7
    その他The residue was purified by column chromatography

実験手順

The compound was synthesized starting from 1-(1H-benzo[d]imidazol-5-yl)-5-(4-(4-oxocyclohexyl)phenyl)pyrrolidine-2,4-dione (1.5 g, 3.87 mmol) and thionyl chloride (1.1 g, 9.1 mmol) according to method 6 described above. The compound was further treated with TFA (5 ml) at room temperature for 1 h. The volatiles were evaporated and the residue was partitioned between sodium bicarbonate solution and MeOH/CHCl3 (5/95). The organic layer was washed with brine, dried over Na2SO4 and evaporated. The residue was purified by column chromatography to give the title compound.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08530670B2uspto-grants-2013_09