HCID 20079496, compound → HCID 15053117, compound

HRID 1654062Notes

Reaction equation

HRID 1654062 reaction equation
[N+:1]([C:4]1[CH:9]=[CH:8][N:7]=[CH:6][C:5]=1[NH:10][C:11]1[CH:12]=[C:13]2[C:17](=[CH:18][CH:19]=1)[NH:16][N:15]=[CH:14]2)([O-])=O>C(O)C>[NH2:1][C:4]1[CH:9]=[CH:8][N:7]=[CH:6][C:5]=1[NH:10][C:11]1[CH:12]=[C:13]2[C:17](=[CH:18][CH:19]=1)[NH:16][N:15]=[CH:14]2

Participants

3

Reactant 1

HCID 20079496HCID 20079496, compound

Product 1

HCID 15053117HCID 15053117, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A suspension of N-(4-nitro-3-pyridinyl)-1H-indazol-5-amine, N5 -oxide (7 g) in 250 ml ethanol containing 0.5 g platinum oxide was hydrogenated at 60 psi for sixty hours and thereafter filtered through Celite and concentrated to 3.3 g solid. This solid was purified by HPLC (silica, 25% methanol in dichloromethane) to give 2.1 g solid. This solid was recrystallized twice from acetonitrile to give 1.5 g crystals, m.p. 198°-199°

Workup

  1. filtrationfiltered through Celite
  2. concentrationconcentrated to 3.3 g solid
  3. customThis solid was purified by HPLC (silica, 25% methanol in dichloromethane)

Sources & evidence

ORD record
ord-13f5cd1747cc41fab292b11325cd3e34
Source dataset
uspto-grants-1995_04
Patent number
US05405856

Reaction notes

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