HuagongsheHuagongshe Chemistry Print Report · For research reference only
9-Bromofluorene → 9-azido-9H-fluorene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 9-Bromofluorene | HCID 16024 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Solvent | Acetone | HCID 180 | — |
| Solvent | Water | HCID 962 | — |
| Product | 9-azido-9H-fluorene | HCID 4330085 | 87.5% |
Reaction Steps
9-Bromo-9H-fluorene (1.00 g, 4.08 mmol) was dissolved in acetone (7 mL). To this was added a solution of NaN3 (1.33 g, 20.4 mmol) in H2O (3 mL). The resulting solution was stirred overnight. Acetone was removed by concentration under reduced pressure. The resulting aqueous mixture was extracted with CH2Cl2 (2×15 mL), and the organic layers were combined, dried over Na2SO4(s), filtered, and concentrated under reduced pressure. The resulting solid residue was purified by silica gel flash chromatography, eluting with hexanes, to give azide 2j as a white solid (0.74 g, 3.57 mmol, 87% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08871916B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-6661303eaa094c25ae818759c7672fe8 |
| Source note | uspto-grants-2014_10 |