Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Piperidine | HCID 8082 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 2-Bromo-4-fluoro-1-nitrobenzene | HCID 2756993 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 66586828 | HCID 66586828 | — |
Reaction Steps
Into a 1000-mL round-bottom flask, was placed a solution of 2-bromo-4-fluoro-1-nitrobenzene (30 g, 137.61 mmol, 1.00 equiv) in N,N-dimethylformamide (450 mL), piperidine (13.974 g, 162.68 mmol, 1.20 equiv), and potassium carbonate (56.718 g, 411.00 mmol, 2.99 equiv). The resulting solution was stirred overnight at 75° C. in an oil bath. The solids were filtered out. The resulting mixture was concentrated under vacuum. The resulting solution was diluted with 300 mL of dichloromethane. The resulting mixture was washed with 2×100 mL of water and 2×100 mL of brine. The mixture was dried over anhydrous sodium sulfate and concentrated under vacuum. The residue was applied onto a silica gel column and eluted with ethyl acetate/petroleum ether (1:50). This resulted in 19 g (49%) of 1-(3-bromo-4-nitrophenyl)piperidine as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08916569B2 |
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| Source dataset | uspto-grants-2014_12 |
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| ORD ID | ord-cbb92af5d3434a1eb3208bf4d3084570 |
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| Source note | uspto-grants-2014_12 |
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