HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,8-Diazabicyclo(5.4.0)undec-7-ene → HCID 58496628, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | P,P-Diphenylphosphinic azide | HCID 199401 | — |
| Reactant | HCID 14994241 | HCID 14994241 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 58496628 | HCID 58496628 | 54.6% |
Reaction Steps
A solution of 1-[4-(trifluoromethyl)phenyl]butan-1-ol (1.4 , 6.4 mmol) and diphenylphosphoryl azide (2.8 ml, 12.8 mmol) in THF (6 mL) cooled to −10° C. under N2 was treated with DBU (1.9 mL, 12.8 mmol). The resulting solution was stirred at room temperature for 20 hours and then diluted with a mixture of ether and H2O. The organic phase was dried and concentrated and the residue purified by column chromatography using hexane:diethyl ethyl acetate (10:1) as eluent to furnish pure azide (0.85 g, 54%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08084456B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-aa2da689746843a5af284e8e75f84673 |
| Source note | uspto-grants-2011_12 |