HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Sulfate → 3-{3-[(3-Methylpiperidin-1-yl)methyl]phenoxy}propan-1-amine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Sulfate | HCID 24436 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 3-[(3-Methylpiperidin-1-yl)methyl]phenol | HCID 13364666 | — |
| Edukt | Aluminium lithium hydride | HCID 21226445 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Diethyl Ether | HCID 3283 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 3-{3-[(3-Methylpiperidin-1-yl)methyl]phenoxy}propan-1-amine | HCID 14026188 | — |
Reaktionsschritte
5.13 g (0.025 mol) of 3-[(3-Methylpiperidin-1-yl) methyl]phenol are introduced into a suspension of 1.0 g (0.025 mol) of sodium hydride (60%) in absolute DMF and stirred overnight at room temperature. After the addition of 2.23 g (0.025 mol) of 3-chloropropionic acid nitrile, the reaction mixture is stirred for 7 hours at 60° C. and then poured into ice water and extracted with ether, and the organic phase is washed with 5% NaOH. After dehydration over Na2SO4, the ethereal phase is introduced dropwise into a suspension of 1.14 g (0.03 mol) of LiAlH4 in absolute ether and then hydrolysed with 2.2 ml of H2O. After filtration and removal of solvent by evaporation under vacuum, 2.96 g of a pale yellow oil are left behind.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04727081 |
| Quelldatensatz | uspto-grants-1988_02 |
| ORD ID | ord-055eb18c1384484c97946551c03e5d3e |
| Quellennotiz | uspto-grants-1988_02 |