Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonium formate | HCID 2723923 | — |
| Reactant | HCID 63363216 | HCID 63363216 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 63362875 | HCID 63362875 | — |
Reaction Steps
To a solution of 6-chloro-N-(2,4-dimethoxybenzyl)pyridazin-3-amine (7.5 g, 26.9 mmol) in ethanol (250 mL) was added ammonium formate (5.94 g, 94.15 mmol) and the mixture was degassed with nitrogen three times. Palladium on charcoal (10 wt %, 2.14 g) was added and the mixture was degassed and recharged with nitrogen and stirred at 80° C. for 90 minutes under a nitrogen atmosphere. The mixture was filtered, concentrated to 15 mL and partitioned between DCM (200 mL) and water (150 mL). The organic layer was washed with brine (150 mL) and concentrated in vacuo. The residue was recrystallised from EtOAc to afford the title compound as cream coloured solid (4.5 g, 68%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09067922B2 |
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| Source dataset | uspto-grants-2015_06 |
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| ORD ID | ord-4c079de8402746d8a2782f805b22c066 |
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| Source note | uspto-grants-2015_06 |
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