Hydrochloric Acid → HCID 178466773, compound

HRID 333637Notes

Reaction equation

HRID 333637 reaction equation
[OH-].[K+].[C:3]([C:6]1[CH:11]=[CH:10][C:9]([N:12]=[N:13][C:14](=[C:18]2[C:27]3[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=3)[CH2:21][C:20]([CH3:29])([CH3:28])[NH:19]2)[C:15](N)=[O:16])=[CH:8][CH:7]=1)(=[O:5])[CH3:4].C([OH:32])C.Cl>O>[C:3]([C:6]1[CH:7]=[CH:8][C:9]([N:12]=[N:13][C:14](=[C:18]2[C:27]3[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=3)[CH2:21][C:20]([CH3:28])([CH3:29])[NH:19]2)[C:15]([OH:32])=[O:16])=[CH:10][CH:11]=1)(=[O:5])[CH3:4]

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 14797Potassium HydroxideHCID 178466770HCID 178466770, compound

Product 1

HCID 178466773HCID 178466773, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

Potassium hydroxide and 2-(4-acetyl-phenylazo)-2-(3,3-dimethyl-3,4-dihydro-2H-isoquinoline-1-ylidene)-acetamide (Asinex Corp., Russia) are added to ethanol, and the mixture is refluxed under heating. The refluxed product is cooled to room temperature and, then, added with distilled water, and further added with hydrochloric acid to make the pH neutral, followed by extracting the reaction product with diethylether. The reaction product is dried by using anhydrous sodium sulfate and filtered and, then, the solvent is removed by reducing the pressure. The residue containing the reaction product is purified by column chromatography to obtain the title compound.

Workup

  1. temperaturethe mixture is refluxed
  2. temperatureunder heating
  3. extractionby extracting the reaction product with diethylether
  4. customThe reaction product is dried
  5. filtrationfiltered
  6. customthe solvent is removed
  7. additionThe residue containing the reaction product
  8. customis purified by column chromatography

Sources & evidence

ORD record
ord-e54fb34d2099484eb3d67f8e804742b1
Source dataset
uspto-grants-2014_11
Patent number
US08883504B2

Reaction notes

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