HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrazine hydrate (1:1) → HCID 59850178, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | HCID 59850172 | HCID 59850172 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 59850178 | HCID 59850178 | 97.2% |
Reaction Steps
A stirred suspension of 1,1-dimethylethyl 4-{[5-bromo-2-nitro-4-(trifluoromethyl)phenyl]amino}-1-piperidinecarboxylate (D66, 1.10 g, 2.3 mmol) in ethanol (50 ml) at room temperature under argon was treated with Raney Nickel (30 mg) followed by dropwise addition over 10 minutes of hydrazine hydrate (0.50 ml, 16 mmol). The mixture was stirred well at room temperature for 20 minutes, then heated at 45° C. for 1 hr, before cooling to 20° C. and filtering through Kieselguhr. The filtrate was concentrated under vacuum to afford the title compound as a white solid (0.98 g, 95%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08288412B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-5470bc672a984b41ae3ddc58333ba476 |
| Source note | uspto-grants-2012_10 |