Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 86689348 | HCID 86689348 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 56942880 | HCID 56942880 | 20.7% |
Reaction Steps
To a 20 ml volume three-necked flask, 1-benzyl-1-(2-(2,6-diethyl-4-methylphenyl)-2-oxoacetyl)-2-(1-methylsulfonyl-2-propylidene)hydrazine ((4-34)-(7)-39) (340 mg), toluene (3.0 ml), and potassium carbonate (0.18 g) were added at room temperature, then additional toluene (0.5 ml) was added. The resulting mixture was stirred at room temperature for 15 hours, then at the internal temperature of about 50° C. for 18 hours. To the resulting mixture, water was added was extracted with tert-butyl methyl ether. The organic layer was concentrated under reduced pressure, purified by column chromatography (hexane: ethyl acetate=5:1), further recrystallized from ethyl acetate to give 67.5 mg of 2-benzyl-4-(2,6-diethyl-4-methylphenyl)-6-methyl-5-methylsulfonyl-2,3-dihydro-3-pyridazinone ((2-34)-(7)-39).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09040709B2 |
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| Source dataset | uspto-grants-2015_05 |
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| ORD ID | ord-b9dd57100f5f4aa389225cfb263f6be3 |
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| Source note | uspto-grants-2015_05 |
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