HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Tert-Butylamine → 1-tert-Butyl-4-piperidone
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Tert-Butylamine | HCID 6385 | — |
| Edukt | 1,1-Dimethyl-4-oxopiperidin-1-ium iodide | HCID 11149497 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 1-tert-Butyl-4-piperidone | HCID 73840 | 4,6% |
Reaktionsschritte
A suspension of 64.5 g (253 mmol) of 1,1-dimethyl-4-oxo-piperidinium iodide in 50 mL of water and 90 mL (860 mmol) of tert-butylamine was stirred for 15 min when 1.0 mL of 40% Triton B in MeOH was added. The mixture was refluxed for 2 hr under N2, and then it was extracted with Et2O (4×100 mL). The aqueous phase was basified with 20 g of NaOH in 20 mL of water, and then it was extracted further with Et2O (4×100 mL). The combined organic extracts were washed with brine, dried over MgSO4, filtered, and concentrated. The residual oil was shaken with 1.5 L of petroleum ether, which was decanted and concentrated. The residue was distilled under vacuum to provide 1.8 g of 1-tert-butyl-piperid-4-one.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07214802B2 |
| Quelldatensatz | uspto-grants-2007_05 |
| ORD ID | ord-fa7946acf03d44b8b7daa22ae543d63e |
| Quellennotiz | uspto-grants-2007_05 |