Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1-(m-Tolyl)piperazine | HCID 83111 | — |
| Reactant | N-(6-Chloropyridazin-3-yl)acetamide | HCID 19095604 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 19814216 | HCID 19814216 | 6.6% |
Reaction Steps
A mixture of 3.5 parts of N-(6-chloro-3-pyridazinyl)acetamide, 3.6 parts of 1-(3-methylphenyl)piperazine and 2.8 parts of potassium carbonate was stirred for 7 hours in an oil bath at 160° C. After cooling, trichloromethane and water were added. The layers were separated. The organic layer was dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (97:3 by volume) as eluent. The second fraction was collected and the eluent was evaporated. The residue was converted into the hydrochloride salt in 2-propanol and 2-propanone. The salt was filtered off and dried, yielding 0.5 parts (6.6%) of 6-[4-(3-methylphenyl)-1-piperazinyl]-3-pyridazinamine dihydrochloride; mp. 178.5° C. (compound 220).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05157035 |
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| Source dataset | uspto-grants-1992_10 |
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| ORD ID | ord-e82bdf66362d4d1c8741897370f57d8f |
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| Source note | uspto-grants-1992_10 |
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