Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | HCID 18977185 | HCID 18977185 | — |
| Reactant | Acetic Acid Mixture with Hydrobromic Acid | HCID 21893785 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 18977156 | HCID 18977156 | 69.6% |
Reaction Steps
44 ml of a 25% hydrogen bromide-acetic acid solution was added to 44 ml of an acetic acid solution containing 2.20 g of 6-[4-(4-aminobutyl)phenyl]-4,5-dihydro-4,5-dimethylpyridazin-3(2H)-one, and the mixture was stirred at room temperature for 5 minutes. Then, 0.75 ml of dimethylsulfoxide was added to the mixture, and the resulting mixture was stirred for 6 hours. The solvent was removed, and the residue was dissolved in 150 ml of water. The solution was made alkaline with ammonia and extracted with chloroform. After the chloroform layer was washed with water and dried, the solvent was removed. The residue was purified by silica gel column chromatography (eluent: chloroform-methanol-28% aqueous ammonia (10:1:0.1)) to obtain 1.52 g of 6-[4-(4-aminobutyl)phenyl]-4,5-dimethylpyridazin-3(2H)-one.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05808065 |
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| Source dataset | uspto-grants-1998_09 |
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| ORD ID | ord-e189b14cd8bb46728961700f4048d6b4 |
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| Source note | uspto-grants-1998_09 |
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