HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
2-Pyrrolidone → 1-(1,4-Dioxaspiro[4.5]decan-8-yl)pyrrolidin-2-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 2-Pyrrolidone | HCID 12025 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 1,4-Dioxaspiro(4.5)decan-8-yl methanesulfonate | HCID 14966741 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 1-(1,4-Dioxaspiro[4.5]decan-8-yl)pyrrolidin-2-one | HCID 10900293 | 11,5% |
Reaktionsschritte
Pyrrolidin-2-one (720 mg, 8.46 mmol) in DMF (5 mL) was treated with NaH (203 mg, 8.46 mmol) at room temperature. The mixture allowed to stir for 30 min. 1,4-dioxaspiro[4.5]decan-8-yl methanesulfonate (500 mg, 2.12 mmol) from above step A, in DMF (3 mL) was added to the mixture and stirred at 130° C. for 3 h. The mixture was cooled to room temperature, quenched with NH4Cl, and extracted into EtOAc. Washed the EtOAc layer with saturated NaCl, dried over Na2SO4 and evaporated. Purified by silica prep TLC to give 55 mg (11.5%) of 1-(1,4-dioxaspiro[4.5]decan-8-yl)pyrrolidin-2-one.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08518969B2 |
| Quelldatensatz | uspto-grants-2013_08 |
| ORD ID | ord-2ce2d8c96c8d4a18932ee09386df8c9e |
| Quellennotiz | uspto-grants-2013_08 |