HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylhydrazine → 1-Methyl-1,5,6,7-tetrahydro-4H-indazol-4-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylhydrazine | HCID 6061 | — |
| Reactant | 2-[(Dimethylamino)methylidene]cyclohexane-1,3-dione | HCID 359353 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 1-Methyl-1,5,6,7-tetrahydro-4H-indazol-4-one | HCID 2765796 | 89.3% |
Reaction Steps
A solution of 46.1 g (1.0 mol) of methylhydrazine in 400 ml of methanol is slowly added dropwise at ambient temperature to a solution of 167.2 g (1.0 mol) of 2-(dimethylaminomethylene)-cyclohexane-1,3-dione in 2000 ml of methanol. The reaction mixture is then refluxed for 1.5 hours. It is evaporated dryness in vacuo and the crude product obtained is purified by chromatography on silica gel (made by Baker, 30-60 μm) with a mixture of ethyl acetate and cyclohexane=9:1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05468766 |
| Source dataset | uspto-grants-1995_11 |
| ORD ID | ord-f8c27671b78c49e7a431f3776f2924a6 |
| Source note | uspto-grants-1995_11 |