Hydroxyamine hydrochloride → HCID 136381053, compound

HRID 1251238Notes

Reaction equation

HRID 1251238 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-ae2e3cacf4ef4e68b110788b5e35aa3c
Source dataset
uspto-grants-2002_01
Patent number
US06340759B1

Reaction notes

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