Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Piperazine | HCID 4837 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 4,5-Dichloro-2-(4-chlorophenyl)-3(2H)-pyridazinone | HCID 779402 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 58585369 | HCID 58585369 | — |
Reaction Steps
55.1 g (200 mmol) of 2-(4-chlorophenyl)-4,5-dichlorpyridazin-3-one are introduced with 41.6 ml (300 mmol) of triethylamine in 400 ml of dimethylformamide. 137.82 g (1600 mmol) of piperazine are added, and the mixture is stirred at 80° C. overnight. The reaction mixture is cooled and then concentrated under high vacuum. The residue is taken up in dichloromethane and washed twice with water, dried over magnesium sulfate and concentrated. The product is isolated by chromatography (gradient: dichloromethane/methanol from 95:5 to 9:1) on silica gel and subsequent crystallization with ether.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07320977B2 |
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| Source dataset | uspto-grants-2008_01 |
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| ORD ID | ord-b4afcbf2ba134864a016e95d442dfcd4 |
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| Source note | uspto-grants-2008_01 |
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