Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Carbon Disulfide | HCID 6348 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | 3-Hydrazinyl-6-(1-methyl-1H-pyrazol-4-yl)pyridazine | HCID 58075172 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178480034 | HCID 178480034 | 77.3% |
Reaction Steps
To a solution of 3-hydrazinyl-6-(1-methyl-1H-pyrazol-4-yl)pyridazine (53 g, 278.6 mmol) in ethanol (550 ml) is added an aqueous solution of KOH (17.2 g, 306.6 mmol) in water (130 mL), followed by CS2 (36 mL, 596.7 mmol). The mixture is stirred at 60-67° C. for 3 h under N2 atmosphere and cooled to RT. Solvents are removed under vacuum and the residue is dissolved in 1N aqueous NaOH (350 mL). The insolubles are filtered off and the filtrate is acidified to pH 2-3 with 1N aqueous HCl. The precipitate is collected, washed with water, and dried under vacuum to provide the title compound (50 g, 77.3%). MS (m/z): 233.0 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08268836B2 |
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| Source dataset | uspto-grants-2012_09 |
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| ORD ID | ord-d71e9ac7fb8d43c09d0fc93519d51ec1 |
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| Source note | uspto-grants-2012_09 |
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