Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrazine | HCID 9321 | — |
| Reactant | HCID 57929962 | HCID 57929962 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 57929956 | HCID 57929956 | 95.5% |
Reaction Steps
A flask was charged with 3-chloro-6-((2,4-difluorophenyl)ethynyl)pyridazine (1.60 g, 6.38 mmol) and 1,4-dioxane (15 mL) to give a tan solution. Anhydrous hydrazine (2.00 mL, 63.8 mmol) was added and the mixture was heated at about 80° C. for about 1 h. The mixture was cooled to ambient temperature and was concentrated in vacuo to about half the original volume. Water (20 mL) was added, followed by sonication, and filtration. The solids were collected and dried in a vacuum oven overnight at about 50° C. to afford the title compound (1.50 g, 95%): LC/MS (Table 1, Method b) Rt=1.72 min; MS m/z: 247.1 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08188083B2 |
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| Source dataset | uspto-grants-2012_05 |
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| ORD ID | ord-b8fc5ca4fda240b7a6cb330a85b77787 |
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| Source note | uspto-grants-2012_05 |
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