Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Ethanol sodium ethoxide | HCID 23706232 | — |
| Reactant | HCID 66602907 | HCID 66602907 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 66602913 | HCID 66602913 | 56% |
Reaction Steps
To 23 ml of ethanol solution containing 1.06 g (2.42 mmol) of 2-bromo-3-bromomethyl-1-(2-trimethylsilylethoxymethyl)-1,5-dihydropyrrolo[2,3-d]pyridazin-4-one obtained in Reference example 24-(f) was added 3.33 g (9.78 mmol) of 20% sodium ethoxide ethanol solution, and the mixture was stirred at room temperature for 1 hour. After completion of the reaction, water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer after separation was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The obtained residue was applied to silica gel column chromatography (Eluent; hexane:ethyl acetate=2:1→1:1 (V/V)), and the fractions containing the desired compound were concentrated under reduced pressure to obtain 549 mg of the title compound as a white solid. (Yield: 56%)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08450319B2 |
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| Source dataset | uspto-grants-2013_05 |
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| ORD ID | ord-c18b6f3234734141a1c5a580272386b3 |
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| Source note | uspto-grants-2013_05 |
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