Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | HCID 25096959 | HCID 25096959 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178441965 | HCID 178441965 | 71% |
Reaction Steps
To a mixture of 5-cyclohexyl-4-(2,2-dimethylpropionoyl)-3-hydroxy-1-(4-isoxazol-3-ylphenyl)-1,5-dihydropyrrol-2-one (0.10 g, 0.25 mmol) and acetic acid (1 mL) was added hydrazine monohydrate (0.036 mL, 0.75 mmol). The mixture was stirred at 85° C. for 3 hr. Water (80 mL) was added to the mixture, which was then extracted with ethyl acetate (100 mL). The organic layer was washed with saturated aqueous sodium bicarbonate (80 mL×2), dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/n-hexane). The crude product was recrystallized from ethyl acetate to give 3-tert-butyl-4-cyclohexyl-5-(4-isoxazol-3-ylphenyl)-4,5-dihydro-1H-pyrrolo[3,4-c]pyrazol-6-one (0.072 g, 71%) as colorless crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08101644B2 |
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| Source dataset | uspto-grants-2012_01 |
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| ORD ID | ord-3b59665357c8466e8c17fd7dba280357 |
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| Source note | uspto-grants-2012_01 |
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