Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Trimethylamine | HCID 1146 | — |
| Reactant | HCID 15079011 | HCID 15079011 | — |
| Reactant | HCID 86754298 | HCID 86754298 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 86754297 | HCID 86754297 | 81.5% |
Reaction Steps
A mixture comprising 1.6 g of 3-[4-(4-aminobenzyl)piperazin-1-yl]-carbonylmethoxy-4-methoxybenzylamine, 770 mg of 4,5-dichloro-6-isopropoxy-3(2H)-pyridazinone, 460 mg of trimethylamine and 20 ml of methanol, was refluxed under heating with stirring for 2 days. The solvent was distilled off under reduced pressure, and the residue was extracted with chloroform. The organic layer was washed with an aqueous potassium carbonate solution and then dried over anhydrous sodium sulfate. Then, the solvent was distilled off. The obtained residue was purified by silica gel column chromatography (ethyl acetate:methanol=9:1→chloroform:methanol=15:1) and then crystallized from diethyl ether to obtain 1.6 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-85486e40219445e7b5ecab00f6681310 |
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| Source note | uspto-grants-1999_07 |
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