HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrazine hydrate (1:1) → (4,5,6,7-Tetrahydro-1H-indazol-5-yl)-carbamic acid tert-butyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | HCID 67317686 | HCID 67317686 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | (4,5,6,7-Tetrahydro-1H-indazol-5-yl)-carbamic acid tert-butyl ester | HCID 67316380 | 55.3% |
Reaction Steps
Hydrazine monohydrate (0.11 mL, 2.35 mmol) was added to a solution of tert-butyl {3-[(dimethylamino)methylene]-4-oxocyclohexyl}carbamate obtained in Example (242a) (526 mg, 1.96 mmol) in methanol (10 mL), and the mixture was heated under reflux for 18 hours. The reaction solution was concentrated. The resulting residue was azeotropically distilled with toluene and then purified by silica gel column chromatography (elution solvent: dichloromethane/methanol 20/1) to obtain 257 mg of the title compound as an amorphous compound (55%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08927588B2 |
| Source dataset | uspto-grants-2015_01 |
| ORD ID | ord-51a474c8e5c4438c852d0871ff93661a |
| Source note | uspto-grants-2015_01 |