Hydrochloric Acid → HCID 13369865, compound

HRID 358507Notes

Reaction equation

HRID 358507 reaction equation
C([N:8]1[CH2:13][CH2:12][N:11]([C:14]([C:16]2[CH:17]=[C:18]3[C:23](=[CH:24][CH:25]=2)[NH:22][C:21](=[O:26])[CH:20]=[CH:19]3)=[O:15])[CH2:10][CH2:9]1)C1C=CC=CC=1.[ClH:27]>[C].[Pd].C(O)C.O>[ClH:27].[N:11]1([C:14]([C:16]2[CH:17]=[C:18]3[C:23](=[CH:24][CH:25]=2)[NH:22][C:21](=[O:26])[CH:20]=[CH:19]3)=[O:15])[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]1

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 13369866HCID 13369866, compound

Product 1

HCID 13369865HCID 13369865, compound

Reagents, catalysts & solvents 2

HCID 178418390HCID 178418390, compoundCatalystHCID 19096565Water ethanolSolvent

Procedure

26.4 Grams of 6-[(4-benzyl-1-piperazinyl)carbonyl]carbostyril was suspended in 800 ml of a mixed solvent of ethanol-water and the pH of the suspension was adjusted to about pH 1 by adding concentrated hydrochloric acid. To this mixture was added 2.6 g of 5% palladium-carbon and catalytic reduction was conducted under a normal pressure at 45°-65° C. After the reaction was completed, the catalyst was removed by filtration and the solvent was removed by distillation under a reduced pressure. The residue obtained was crystallized by adding acetone and the crude crystals thus obtained were recrystallized from ethanol-water to obtain 19.9 g of 6-(1-piperazinylcarbonyl)carbostyril monohydrochloride. Colorless granular crystals. Melting point: over 300° C.

Workup

  1. customwas conducted under a normal pressure at 45°-65° C
  2. customthe catalyst was removed by filtration
  3. customthe solvent was removed by distillation under a reduced pressure
  4. customThe residue obtained
  5. customwas crystallized
  6. additionby adding acetone
  7. customthe crude crystals thus obtained
  8. customwere recrystallized from ethanol-water

Sources & evidence

ORD record
ord-ea5d96c5a0f64f319ffcd4286d5555a0
Source dataset
uspto-grants-1984_08
Patent number
US04468402

Reaction notes

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