反応 #507713
ord-d123f979ed164afcbff9362187f050c5
反応方程式
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1抽出extracted with DCM (5×)
- 2乾燥The combined organic fractions were dried over Na2SO4
- 3ろ過filtered
- 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.