HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → cis-Tert-butyl 3-azido-4-fluoropiperidine-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | trans-Tert-butyl 4-fluoro-3-(tosyloxy)piperidine-1-carboxylate | HCID 131729717 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | cis-Tert-butyl 3-azido-4-fluoropiperidine-1-carboxylate | HCID 131729718 | 54.1% |
Reaction Conditions
| Temperature | 128 °C |
|---|
Reaction Steps
A mixture of trans-tert-butyl 4-fluoro-3-(tosyloxy)piperidine-1-carboxylate (3.95 g, 10.6 mmol) and NaN3 (1.72 g, 26.4 mmol) in DMF (30 mL) was stirred at 128° C. (bath) for 18 hours. After cooling to room temperature, ether (100 mL) was added. The mixture was washed with brine (2×50 mL), dried (sodium sulfate) and concentrated in vacuo. The residue obtained was purified by flash chromatography on silica gel (hexane:ethyl acetate 4:1) to give cis-tert-butyl 3-azido-4-fluoropiperidine-1-carboxylate (1.40 g, 54%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08178131B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-265e7dc851ba48f8b4af85e900792eff |
| Source note | uspto-grants-2012_05 |