HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Imidazole → HCID 178455374, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Imidazole | HCID 795 | — |
| Edukt | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| Edukt | HCID 178521634 | HCID 178521634 | — |
| Katalysator | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | HCID 178455374 | HCID 178455374 | 73,1% |
Reaktionsschritte
To a solution of cis-3-(benzyloxymethyl)cyclobutanol (Albany Molecular, 1.0 g, 5.2 mmol) in CH2Cl2 (20 mL) was added imidazole (0.71 g, 10.4 mmol), DMAP (64 mg, 0.52 mmol) and tert-butyldimethylsilylchloride (TBSCl) (1.6 g, 10.4 mmol). This mixture was stirred at ambient temperature for 16 h, quenched with saturated, aqueous NH4Cl (5 mL) and diluted with EtOAc (10 mL). The layers were separated and the aqueous layer was extracted with EtOAc (3×5 mL). The combined organics were dried over anhydrous Na2SO4, filtered, concentrated under reduced pressure and purified via column chromatography (SiO2, 50% hexanes/EtOAc) to give the title compound (1.15 g, 3.8 mmol, 72% yield). MS (DCI/NH3) m/z 307 (M+H)+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08492371B2 |
| Quelldatensatz | uspto-grants-2013_07 |
| ORD ID | ord-f5f9a21780be44ee94d657912589e32e |
| Quellennotiz | uspto-grants-2013_07 |