Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 4,5-Dichloro-3-hydroxypyridazine | HCID 73247 | — |
| Reactant | 3-(4-Methylpiperazin-1-yl)-carbonylmethoxy-4-methoxybenzylamine | HCID 86754292 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 86754293 | HCID 86754293 | 47.9% |
Reaction Steps
A mixture comprising 1.16 g of 3-(4-methylpiperazin-1-yl)-carbonylmethoxy-4-methoxybenzylamine, 0.5 g of 4,5-dichloro-3(2H)-pyridazinone, 0.46 g of triethylamine, 10 ml of ethanol and 10 ml of water, was refluxed under heating with stirring overnight. The solvent was distilled off under reduced pressure, and an aqueous potassium carbonate solution was added to the residue. The mixture was extracted with chloroform. The extract solution was washed with water and a saturated sodium chloride aqueous solution and then dried over anhydrous sodium sulfate. Then, the solvent was distilled off. The obtained residue was purified by silica gel column chromatography and then crystallized from chloroform/diethyl ether to obtain 0.61 g of the above-identified compound as white crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05929074 |
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| Source dataset | uspto-grants-1999_07 |
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| ORD ID | ord-9eee5d55776a4bcfbc8c29cfab6e60d5 |
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| Source note | uspto-grants-1999_07 |
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