HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Imidazole → HCID 178434091, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Imidazole | HCID 795 | — |
| Edukt | Dichloromethane | HCID 6344 | — |
| Edukt | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| Edukt | HCID 178434090 | HCID 178434090 | — |
| Katalysator | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Produkt | HCID 178434091 | HCID 178434091 | — |
Reaktionsschritte
A mixture of trans-4-(4-iodo-3,5-dimethyl-1H-pyrazol-1-yl)cyclohexanol (206.0 mg, 0.6434 mmol), tert-butyldimethylsilyl chloride (0.194 g, 1.29 mmol), 4-dimethylaminopyridine (20 mg, 0.1 mmol), imidazole (131 mg, 1.93 mmol) and DCM (4 mL, 60 mmol) was stirred at rt for 20 min. The material was transferred to a separatory funnel, extracting with DCM and sat. NaHCO3. The organic layer was dry-loaded onto silica gel for column chromatography, eluting with 3% EtOAc/hexanes. The fractions containing the pure product were concentrated in vacuo to afford the title compound as a clear oil. MS (ES+): m/z=435.14 (100) [MH+]. HPLC: tR=2.26 min (polar—3 min, UPLC-ACQUITY).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08445510B2 |
| Quelldatensatz | uspto-grants-2013_05 |
| ORD ID | ord-a634e5163c8842a0b136b1f00951aa35 |
| Quellennotiz | uspto-grants-2013_05 |