HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → (S)-N-(2,3-dihydro-7H-1,4-dioxino[2,3-e]indazol-2-ylmethyl)-1-[1-(2-methoxyphenyl)piperid-4-yl]methylamine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Dimethylformamide | HCID 6228 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | (1-(2-Methoxyphenyl)piperidin-4-yl)methanamine | HCID 10608971 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | (S)-N-(2,3-dihydro-7H-1,4-dioxino[2,3-e]indazol-2-ylmethyl)-1-[1-(2-methoxyphenyl)piperid-4-yl]methylamine | HCID 22951194 | — |
Reaktionsschritte
A mixture of the product from the previous reaction (0.25 g), potassium carbonate (2 g) and 1-[1-(2-methoxyphenyl)piperid-4-yl]methylamine (0.3 g) in a mixture of dimethylformamide (5 ml) and toluene (10 ml) was heated at reflux temperature for 8 hours. The cooled mixture was poured into water (100 ml) and extracted with ethyl ether (2×100 ml). The combined extracts were then dried over magnesium sulphate and the solvent removed under reduced pressure to yield a yellow oil. Purification by flash column chromatography on silica eluting with a 20:1 mixture of dichloromethane and methanol afforded (S)-N-(2,3-dihydro-7H-1,4-dioxino[2,3-e]indazol-2-ylmethyl)-1-[1-(2-methoxyphenyl)piperid-4-yl]methylamine (0.04 g) as a gummy solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06353002B2 |
| Quelldatensatz | uspto-grants-2002_03 |
| ORD ID | ord-fcda2ad889ac400fae83987b1196b19a |
| Quellennotiz | uspto-grants-2002_03 |