Hydroxyamine hydrochloride → HCID 136381053, compound

HRID 1006996Notes

Reaction equation

HRID 1006996 reaction equation
[CH2:1]([N:3]1[CH2:8][CH2:7][N:6]([C:9]2[C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[CH:12]=[C:11]([C:19]3[CH:24]=[CH:23][C:22]([C:25](=O)[CH2:26][CH2:27][CH3:28])=[CH:21][CH:20]=3)[N:10]=2)[CH2:5][CH2:4]1)[CH3:2].Cl.[NH2:31][OH:32].C([O-])(=O)C.[Na+]>C(O)C.O>[CH2:1]([N:3]1[CH2:8][CH2:7][N:6]([C:9]2[C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[CH:12]=[C:11]([C:19]3[CH:24]=[CH:23][C:22]([C:25](=[N:31][OH:32])[CH2:26][CH2:27][CH3:28])=[CH:21][CH:20]=3)[N:10]=2)[CH2:5][CH2:4]1)[CH3:2]

Participants

6

Reactant 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 22502626HCID 22502626, compound

Product 1

HCID 136381053HCID 136381053, compoundYield 82%

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent

Procedure

1-(4-Ethylpiperazin-1-yl)-3-(4-butyrylphenyl)isoquinoline (0.27 g) obtained in the previous Example was dissolved in ethanol (40 ml), to which was then added a solution of hydroxylamine hydrochloride (0.14 g) and sodium acetate (0.22 g) dissolved in water (10 ml), and the mixture was heated under reflux. The solvent was evaporated, and the resulting residue was purified by NH-silica gel column chromatography (ethyl acetate/methanol system), to give 0.23 g of the free compound of the title compound as a pale brown amorphous.

Workup

  1. temperaturethe mixture was heated
  2. temperatureunder reflux
  3. customThe solvent was evaporated
  4. customthe resulting residue was purified by NH-silica gel column chromatography (ethyl acetate/methanol system)

Sources & evidence

ORD record
ord-d82cc6f77d6e4918ac056aa877c9e6ae
Source dataset
uspto-grants-2004_09
Patent number
US06790844B2

Reaction notes

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