HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl acetoacetate → 2-Cyclohexyl-5-methyl-2,4-dihydro-pyrazol-3-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl acetoacetate | HCID 7757 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Cyclohexylhydrazine hydrochloride | HCID 207836 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2-Cyclohexyl-5-methyl-2,4-dihydro-pyrazol-3-one | HCID 10192605 | 71% |
Reaction Steps
A mixture solution of 39.88 g (0.265 mol) of cyclohexylhydrazine HCl salt in 28.57 mL (0.265 mol) of methyl acetoacetate was heated for 1 hour at 120° C. After the reaction mixture was cooled to room temperature, dichloromethane was added to this mixture and the mixture was neutralized by 2N—NaOH aqueous solution. The organic layer was dried over with anhydrous sodium sulfate and the solvent was removed under reduced pressure. The resulting residue was treated with hexane to give crystalline and the crystalline was collected by filtration to give 33.84 g (71%) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08901315B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-0fd8304752284b3f8b431a2ac6a1595e |
| Source note | uspto-grants-2014_12 |