HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Phosphorus oxychloride → 2-chloro-6-(trifluoromethyl)-1H-benzimidazole
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Phosphorus oxychloride | HCID 24813 | — |
| Edukt | 5-Trifluoromethyl-1,3-dihydro-benzimidazol-2-one | HCID 11820150 | — |
| Produkt | 2-chloro-6-(trifluoromethyl)-1H-benzimidazole | HCID 337905 | — |
Reaktionsschritte
A solution of the dihydrobenzoimidazol-2-one from step (b) above (2.02 g, 10 mmol) in POCl3 (30 mL) was heated at 95° C. for 16 h. The reaction mixture was cooled to room temperature, the solvent was removed in vacuo and the resulting oily residue subjected to azeotropic distillation with toluene (3×50 mL) at 50° C. The crude product was dissolved in EtOAc (50 mL), washed with brine (10 mL) then dried over Na2SO4 and filtered. The solvent was removed in vacuo and the residue was recrystallized from EtOAc/hexane to give the title compound.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07582761B2 |
| Quelldatensatz | uspto-grants-2009_09 |
| ORD ID | ord-2eaab8ce31e44ef193d5a21e9388dd8c |
| Quellennotiz | uspto-grants-2009_09 |