반응 #3968

ord-f3d5d152d9a34241b654d7e6361c94bd

반응 방정식

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

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도refluxed for 1.75 hours
  2. 2
    농축The reaction mixture is concentrated by evaporation
  3. 3
    기타the residue is triturated with 50 ml of ice water
  4. 4
    기타the product precipitated
  5. 5
    기타is purified by chromatography on silica gel [eluant: methylene chloride/ethanol (100:0 to 100:2)]

실험 절차

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)].

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04722929uspto-grants-1988_02