HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
2-(Trifluoromethoxy)benzoyl Chloride → 2-Trifluoromethoxy-N-[6-(1-methyl-piperidin-4-ylcarbonyl)-pyridin-2-yl]-benzamide mono-hydrochloride salt
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 2-(Trifluoromethoxy)benzoyl Chloride | HCID 2777241 | — |
| Edukt | (6-Aminopyridin-2-yl)(1-methylpiperidin-4-yl)methanone | HCID 11401723 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | 2-Trifluoromethoxy-N-[6-(1-methyl-piperidin-4-ylcarbonyl)-pyridin-2-yl]-benzamide mono-hydrochloride salt | HCID 17980388 | 76% |
Reaktionsschritte
Combine 2-amino-6-(1-methylpiperidin-4-ylcarbonyl)pyridine (0.18 g, 0.84 mmol), 2-trifluoromethoxybenzoyl chloride (0.23 g, 1.0 mmol) and 1,4-Dioxane (5 mL). Stir and heat the mixture at reflux. After 3 hr., cool the reaction mixture to ambient temperature. Load on an SCX column (10 g), wash with methanol, and elute with 2M ammonia/methanol. Concentrate the eluent to obtain the free base of the title compound (0.26 g, 76%). Dissolve the free base in methanol (10 mL) and treat with ammonium chloride (0.032 g). Concentrate and dry under vacuum to obtain the title compound. HRMS Obs. m/z 408.1517, Calc. m/z 408.1535; m.p. 155-160° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07423050B2 |
| Quelldatensatz | uspto-grants-2008_09 |
| ORD ID | ord-ac0f35488146473ea80a7be32996d9f7 |
| Quellennotiz | uspto-grants-2008_09 |