反応 #507713

ord-d123f979ed164afcbff9362187f050c5

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出extracted with DCM (5×)
  2. 2
    乾燥The combined organic fractions were dried over Na2SO4
  3. 3
    ろ過filtered
  4. 4
    その他evaporated to dryness

実験手順

To a solution of 6-(2,4-dichloro-phenyl)-imidazo[1,2-a]pyridine-7-carbonitrile (3.07 g, 6.10 mmol, prepared according to Example 3, Step 2.3) in concentrated H2SO4 (55 mL) was added a freshly prepared mixture of fuming HNO3 in H2SO4 (1:2, v/v, 2.55 mL) at RT. The reaction mixture was stirred at RT for 2 h then cautiously added to cold water (300 mL) and extracted with DCM (5×). The combined organic fractions were dried over Na2SO4, filtered, and evaporated to dryness to give the crude 6-(2,4-dichloro-phenyl)-3-nitro-imidazo[1,2-a]pyridine-7-carbonitrile as a brown solid (533 mg). MS: 333 [M+1]+; HPLC: AtRet=1.57.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08097617B2uspto-grants-2012_01