HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-Nitroaniline → HCID 90052079, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-Nitroaniline | HCID 7423 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | Tert-butyl 3-oxopiperidine-1-carboxylate | HCID 2756825 | — |
| Reactant | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 90052079 | HCID 90052079 | 55.5% |
Reaction Steps
To a solution of 1-Boc-3-piperidinone (256 mg) and 3-nitroaniline (190 mg) in methylene chloride (7 mL), sodium triacetoxyborohydride (438 mg) and acetic acid (80 μL) were added at room temperature, and the mixture was stirred at the same temperature for 15 hours. To the reaction mixture, ethyl acetate and saturated aqueous sodium hydrogencarbonate were added. The organic layer was separated, washed with saturated aqueous sodium chloride, and then dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (eluent, 100 to 50% hexane in ethyl acetate) to obtain tert-butyl 3-((3-nitrophenyl)amino)piperidine-1-carboxylate (C21, 229 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09145415B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-aa2ad9da4e3e4ce1ac429c02e5da2fe4 |
| Source note | uspto-grants-2015_09 |