HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Toluene → HCID 22285400, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Toluene | HCID 1140 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | Bromomethylcyclopropane | HCID 81503 | — |
| Edukt | Ethyl 1,3-dithiane-2-carboxylate | HCID 88552 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | HCID 22285400 | HCID 22285400 | — |
Reaktionsschritte
To a flamed dried flask is added dry toluene (80 mL) and sodium hydride (60%, 33.5 mmol, 1.34 g). The reaction is cooled in a ice bath and a solution of ethyl 1,3 dithiane carboxylate (52 mmol, 10 g) and bromomethyl cyclopropane (62.4 mmol, 8.42 g) in DMF (24 mL) are added dropwise over 10 minutes. The ice bath is removed and the reaction is stirred for 18 h. Water is added (50 mL) and the organic layer is separated. The organic layer is washed with brine, dried (Na2SO4), and concentrated to a yellow oil (12 g, 92%). LC-ES/MS: 247.0 (M+1).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08153624B2 |
| Quelldatensatz | uspto-grants-2012_04 |
| ORD ID | ord-2b7089650b25413781be88d029022323 |
| Quellennotiz | uspto-grants-2012_04 |