Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrogen Bromide | HCID 260 | — |
| Reactant | HCID 13199847 | HCID 13199847 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 15590492 | HCID 15590492 | 69.6% |
Reaction Steps
1.0 g of 5-(2-morpholinobutyryl)-8-hydroxy-3,4-dihydrocarbostyril (IIb) hydrobromide was dissolved in 70 ml of water and 0.2 g of palladium-on-carbon and 0.3 g of palladium black were added to the solution followed by allowing the mixture to catalytically reduce under atmospheric pressure in a hydrogen atmosphere for 10 days at a temperature of 70° C while shaking. After completion of the reduction, the reaction mixture was filtered to remove the catalysts by filtration, and the filtrate was concentrated to dryness under reduced pressure. The resulting residue was dissolved in acetone by heating followed by allowing the solution to cool. The precipitate formed upon cooling was recrystallized from ethanol to obtain 0.7 g of white amorphous 5-(2-morpholino-1-hydroxybutyl)-8-hydroxy-3,4-dihydrocarbostyril (I) hydrobromide 1/2 hydrate having a melting point of 183° - 185° C (with decomposition). The product thus obtained was confirmed by NMR and IR spectral analyses and elemental analysis.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US03994901 |
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| Source dataset | uspto-grants-1976_11 |
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| ORD ID | ord-61c0b6825fcf493a87f7ea493d002383 |
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| Source note | uspto-grants-1976_11 |
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