HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → HCID 22930021, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Edukt | P,P-Diphenylphosphinic azide | HCID 199401 | — |
| Edukt | (6-Ethylpyridin-3-yl)methanol | HCID 22929790 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | HCID 22930021 | HCID 22930021 | 84,5% |
Reaktionsschritte
After dissolving (6-ethyl-3-pyridyl)methanol (2.25 g, 16.4 mmol) in toluene (25 ml), diphenylphosphoryl azide (4.2 ml, 19.6 mmol) and 1,8-diazabicyclo[5.4.0]undec-7-ene (2.9 ml, 19.6 mmol) were added while stirring on ice, and the mixture was further stirred at room temperature for 18 hours. Water was added for treatment and extraction was performed with ethyl acetate. The extract was washed with brine and then dried over sodium sulfate and filtered. The filtrate was concentrated under reduced pressure and the residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate) to yield the title compound (2.2 g) as a yellow oil. (84.5% yield)
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07244730B2 |
| Quelldatensatz | uspto-grants-2007_07 |
| ORD ID | ord-6bcd0e354ba34994a837ebd5e87e3c84 |
| Quellennotiz | uspto-grants-2007_07 |