Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 86590811 | HCID 86590811 | — |
| Catalyst | Silver Nitrate | HCID 24470 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 20725517 | HCID 20725517 | 51% |
Reaction Steps
To a solution of silver nitrate (0.85 g, 5 mmol) in water (2.5 ml) was added an aqueous 2N lithium hydroxide solution (3 ml), followed by a solution of 7-(4-fluorobenzyloxy)-3-formyl-2-methyl-1-[(1S,2S)-2-methylcyclopropylmethyl]pyrrolo[2,3-d]pyridazine (0.177 g, 0.5 mmol) in ethanol (10 ml). The mixture was stirred at room temperature for 48 hours. To the reaction mixture was added 1N hydrochloric acid (3 ml) and the resulting mixture was filtered through celite (trade mark). The celite (trade mark) was washed with ethanol (30 ml). To the combined filtrates was added water and the resulting mixture was extracted with chloroform. The extract was dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was chromatographed on a silica gel column using chloroform/isopropanol=19/1 as the eluant to give the title compound (0.094 g, 51%) as pale yellow crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06734181B2 |
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| Source dataset | uspto-grants-2004_05 |
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| ORD ID | ord-c31c3375d0ea4087a160d2da8e2b928e |
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| Source note | uspto-grants-2004_05 |
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