HuagongsheHuagongshe Chemistry Print Report · For research reference only
Piperazine → 3-Pyridazinamine, 6-(4-methyl-1-piperazinyl)-
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Piperazine | HCID 4837 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 6-Amino-3-chloropyridazine | HCID 21643 | — |
| Reactant | 3-Chloropyridine--hydrogen chloride (1/1) | HCID 18406597 | — |
| Product | 3-Pyridazinamine, 6-(4-methyl-1-piperazinyl)- | HCID 20316816 | 53.6% |
Reaction Steps
An amount of 1.0 g (7.72 mmol) of 3-amino-6-chloropyridazine, 5-chloro pyridine hydrogen chloride (4.46 g, 38.6 mmol), and piperazine (5.1 mL, 72 mmol) were placed in a pre-heated oil bath at 165-170° C. for 4 hours. After cooling, the mixture is basified with saturated potassium carbonate, extracted 3× with ethyl acetate and dried over magnesium sulfate. The oily residue is purified by column chromatography to give a brown solid 800 mg (53% yield). MS (ESI) m/z 194.3 (M+1)+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07713994B2 |
| Source dataset | uspto-grants-2010_05 |
| ORD ID | ord-094ec649dfa144e792abdc6e816c4e94 |
| Source note | uspto-grants-2010_05 |