HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium hydride → Diallyl 2,2-bis(pyrenylmethyl)malonate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 1-(Chloromethyl)pyrene | HCID 97581 | — |
| Edukt | Diallyl malonate | HCID 228227 | — |
| Lösungsmittel | Benzene | HCID 241 | — |
| Produkt | Diallyl 2,2-bis(pyrenylmethyl)malonate | HCID 15361862 | — |
Reaktionsschritte
Diallyl malonate (0.36 g, 2.0 mmol) was added to a stirred suspension of NaH (2.5 mmol) in dry benzene (5 mL). After 30 minutes 1-chloromethylpyrene (0.5 g, 2.0 mmol) in benzene (20 mL) was added. The mixture was gently refluxed for 18 hours, cooled to room temperature and washed with saturated aqueous NaCl (2×5 mL). The organic layer was dried over MgSO4 and the solvent evaporated under reduced pressure to give the product, which was recrystallized from AcOEt/hexane to afford the desired product as white crystals, yield: 0.26 g, 42%, m.p. 178°-180° C. 1H NMR and 13C NMR were in accord with the desired product. Analysis (C43H32O4): calculated C:84.29, H:5.26; found: C:84.13, H:5.23.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05498549 |
| Quelldatensatz | uspto-grants-1996_03 |
| ORD ID | ord-ba8350f7b5e447fa9fd6ad461b4c7783 |
| Quellennotiz | uspto-grants-1996_03 |