HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium hydride → 1-(2,2-Dimethoxyethyl)-piperidin-2-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 5-Chlorovaleryl chloride | HCID 74089 | — |
| Edukt | Aminoacetaldehyde dimethyl acetal | HCID 89728 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Lösungsmittel | Sodium Carbonate | HCID 10340 | — |
| Produkt | 1-(2,2-Dimethoxyethyl)-piperidin-2-one | HCID 21978509 | 80,9% |
Reaktionsschritte
To a stirred mixture of aminoacetaldehyde dimethylacetal (0.74 g, 7 mmole) in ethyl acetate (20 mL) and 2M sodium carbonate (20 mL) was added 5-chlorovaleryl chloride (1.55 g, 10 mmole). The reaction mixture was stirred at ambient temperature for 1 hour. The aqueous layer was separated and extracted with ethyl acetate. The combined organic phase was washed with 1% hydrochloric acid and water, dried (magnesium sulfate), and concentrated. The oily residue was dissolved in tetrahydrofuran, and sodium hydride (60% in oil) (0.3 g, 7.5 mmole) was added. The reaction mixture was heated under reflux for 1.5 hours and filtered. The filtrate was concentrated to give 1-(2,2-dimethoxyethyl)-piperidin-2-one (1.06 g) as a pale yellow oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07094778B2 |
| Quelldatensatz | uspto-grants-2006_08 |
| ORD ID | ord-1a741121a16944648d852fb3d307e1e8 |
| Quellennotiz | uspto-grants-2006_08 |