HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
4-Methylmorpholine → 1-(5-Methyl-2-(pyridin-4-yl)benzoyl)piperidin-4-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 4-Methylmorpholine | HCID 7972 | — |
| Edukt | 4-(4,6-Dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chloride | HCID 2734059 | — |
| Edukt | 4-Piperidone hydrochloride | HCID 3084851 | — |
| Edukt | 5-Methyl-2-(pyridin-4-yl)benzoic acid hydrochloride | HCID 86680842 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 1-(5-Methyl-2-(pyridin-4-yl)benzoyl)piperidin-4-one | HCID 86680848 | 31% |
Reaktionsschritte
A suspension of 5-methyl-2-(pyridin-4-yl)benzoic acid hydrochloride (2.0 g), piperidin-4-one hydrochloride (1.2 g), DMTMM (3.3 g) and N-methylmorpholine (2.6 mL) in DMF (30 mL) was stirred at room temperature for 5 hr, and then overnight at 100° C. The reaction mixture was diluted with water, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (0.73 g).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08648079B2 |
| Quelldatensatz | uspto-grants-2014_02 |
| ORD ID | ord-e5f3a5eb1548437391af722717e65e5d |
| Quellennotiz | uspto-grants-2014_02 |