Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | 1,3-Bis(diphenylphosphino)propane | HCID 81219 | — |
| Reactant | HCID 86600914 | HCID 86600914 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Product | HCID 69331847 | HCID 69331847 | — |
Reaction Steps
A mixture of 5-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-6-phenyl-2-pyrazinyl trifluoromethanesulfonate (1.0 g), MeOH (5.98 ml), palladium acetate (102 mg) and 1,3-bis(diphenylphosphino)propane (187 mg) in DMF (10 ml) was stirred with CO gas bubbling at 20° C. for 30 minutes. Then the reaction mixture was stirred under CO gas at 60° C. for 6 hours. Water and EtOAc were added to the reaction mixture. The organic layer was washed with 1N HCl, aq. NaHCO3 and brine. The organic layer was separated, and dried over MgSO4. The solvent was removed in vacuo. The residue was purified by silica gel column chromatography eluted with a mixture of n-hexane and EtOAc. The fractions were concentrated in vacuo to obtain methyl 5-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-6-phenyl-2-pyrazinecarboxylate (68 mg) as white powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07265120B2 |
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| Source dataset | uspto-grants-2007_09 |
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| ORD ID | ord-403e80e90d3242f18ff76d404557db36 |
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| Source note | uspto-grants-2007_09 |
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