HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1-(6-Methylpyridin-3-yl)ethanamine → 4-Hydroxy-6-methyl-1-[1-(6-methyl-pyridin-3-yl)-ethyl]-1H-pyridin-2-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1-(6-Methylpyridin-3-yl)ethanamine | HCID 45791096 | — |
| Edukt | 4-Hydroxy-6-methyl-2-pyrone | HCID 54675757 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 4-Hydroxy-6-methyl-1-[1-(6-methyl-pyridin-3-yl)-ethyl]-1H-pyridin-2-one | HCID 59603095 | 17,5% |
Reaktionsschritte
A stirred mixture of 4-Hydroxy-6-methyl-2-pyrone (1.394 g, 11.1 mmol) and 1-(6-Methyl-pyridin-3-yl)-ethylamine (1.806 g, 13.3 mmol) in water (18 ml) was boiled under reflux for 65 h. The mixture was cooled to ambient temperature and the supernatant liquid was decanted off to leave a dark semi-solid residue. This was triturated with ethyl acetate to give 4-Hydroxy-6-methyl-1-[1-(6-methyl-pyridin-3-yl)-ethyl]-1H-pyridin-2-one as a grey solid (475 mg) which was used in the next step without further purification. LC-MS m/z 245 [M+H]+ Rt=1.21 min.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08299065B2 |
| Quelldatensatz | uspto-grants-2012_10 |
| ORD ID | ord-2cad03700ab24716b4df40c9c073315c |
| Quellennotiz | uspto-grants-2012_10 |