HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Azide → 2-(2-Azidoethoxy)oxane
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | 2-(2-Bromoethoxy)tetrahydro-2H-pyran | HCID 86621 | — |
| Reactant | Water ethylacetate | HCID 22728543 | — |
| Catalyst | Tetrabutylammonium Iodide | HCID 67553 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 2-(2-Azidoethoxy)oxane | HCID 60074287 | — |
Reaction Steps
A mixture of 2-(2-bromo-ethoxy)-tetrahydro-pyran (1.00 mL, 6.62 mmol), NaN3 (4.34 g, 66 mmol) and tetrabutylammonium iodide (245 mg, 0.66 mmol) in DMF (7.0 mL) was stirred at RT for 18 h. The reaction mixture was poured into a mixture of EtOAc/water. The organic phase was washed with water, brine and then dried (MgSO4), filtered and concentrated in vacuo to give the crude product. The crude product was purified by continuous gradient flash chromatography using EtOAc/petroleum ether (40-60) 0:100 to 20:80 as the eluent to afford the title compound as colourless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08293772B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-ee53d6f9a5bf41f3b026d03b2a71bebc |
| Source note | uspto-grants-2012_10 |