HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 2,9-Diazaspiro(5.5)undecan-1-one hydrochloride
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | tert-Butyl 1-oxo-2,9-diazaspiro[5.5]undecane-9-carboxylate | HCID 49760149 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | 2,9-Diazaspiro(5.5)undecan-1-one hydrochloride | HCID 45074288 | 96% |
Reaktionsschritte
To the stirred solution of tert-butyl 1-oxo-2,9-diazaspiro[5.5]undecane-9-carboxylate (3.0 g, 11.19 mmol) in DCM (60 mL) was added 4N HCl in dioxane (20 mL) and the mixture was stirred at rt for 18 h. The solvent was removed under reduced pressure and triturated with diethyl ether (2×5 mL) to yield the title compound as a solid (2.2 g, 96%). Note: The product is moisture sensitive. [1H-NMR (DMSO-d6, 300 MHz): δ 9.25-8.68 (m, 2H), 7.43 (s, 1H), 7.20-6.25 (m, 2H), 3.61-2.90 (m, 5H), 2.12-1.95 (m, 2H), 1.76-1.49 (m, 5H); LCMS RtA=0.326, [M+H]+=169.0].
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08530648B2 |
| Quelldatensatz | uspto-grants-2013_09 |
| ORD ID | ord-67defb743249464596a605a19e4e499a |
| Quellennotiz | uspto-grants-2013_09 |