反応 #3968

ord-f3d5d152d9a34241b654d7e6361c94bd

反応方程式

COc1ccc2[nH]c(-c3cc([N+](=O)[O-])c(N4C(=O)c5cc([N+](=O)[O-])ccc5C(C)(C)C4=O)cc3OC)nc2n1
2-[2-methoxy-5-nitro-4-(4,4-dimethyl-7-nitro-2H,4H-isoquinolin-1,3-dione-2-yl)-phenyl]-5-methoxy-imidazo[4,5-b]pyridine
NN.O
hydrazine hydrate
COc1ccc2[nH]c(-c3cc([N+](=O)[O-])c(N)cc3OC)nc2n1
2-(2-Methoxy-4-amino-5-nitro-phenyl)-5-methoxy-imidazo[4,5-b]pyridine

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度refluxed for 1.75 hours
  2. 2
    濃縮The reaction mixture is concentrated by evaporation
  3. 3
    その他the residue is triturated with 50 ml of ice water
  4. 4
    その他the product precipitated
  5. 5
    その他is purified by chromatography on silica gel [eluant: methylene chloride/ethanol (100:0 to 100:2)]

実験手順

One half gram of 2-[2-methoxy-5-nitro-4-(4,4-dimethyl-7-nitro-2H,4H-isoquinolin-1,3-dione-2-yl)-phenyl]-5-methoxy-imidazo[4,5-b]pyridine is suspended in 10 ml of isopropanol, mixed with 0.5 ml of 80% hydrazine hydrate, and refluxed for 1.75 hours with stirring. The reaction mixture is concentrated by evaporation, the residue is triturated with 50 ml of ice water, and the product precipitated is purified by chromatography on silica gel [eluant: methylene chloride/ethanol (100:0 to 100:2)].

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04722929uspto-grants-1988_02