HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 2-[4-(2,6-Dichlorophenyl)piperazin-1-yl]-6-trifluoromethyl-1H-benzoimidazole
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | 2-chloro-6-(trifluoromethyl)-1H-benzimidazole | HCID 337905 | — |
| Edukt | 1-(2,6-Dichlorophenyl)piperazine | HCID 11492345 | — |
| Lösungsmittel | Dimethyl Sulfoxide | HCID 679 | — |
| Produkt | 2-[4-(2,6-Dichlorophenyl)piperazin-1-yl]-6-trifluoromethyl-1H-benzoimidazole | HCID 10047447 | — |
Reaktionsschritte
A mixture of the benzoimidazole from step (c) above (75 mg, 0.34 mmol), the piperazine from step (a) above (90 mg, 0.39 mmol) and N,N-diisopropylethylamine (0.1 mL, 0.58 mmol, Aldrich) in DMSO (2 mL) was stirred at 80° C. for 24 h. The mixture was cooled to room temperature, water (10 mL) was added and the mixture was extracted with EtOAc (2×20 mL). The combined organic phases were washed with water (2×10 mL) and brine (5 mL), dried over Na2SO4, and filtered. The solvent was removed in vacuo and the residue was purified by silica gel chromatography, eluting with 20% EtOAc/hexane to give the title compound as a white solid. M.p. 263-265° C. MS (ESI, pos. ion) m/z: 415 (M+1).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07582761B2 |
| Quelldatensatz | uspto-grants-2009_09 |
| ORD ID | ord-18db05cfa2954c4b856ff9818bcadebf |
| Quellennotiz | uspto-grants-2009_09 |