HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → Tropenol 9-hydroxyfluorene-9-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Methyl 9-hydroxy-9H-fluorene-9-carboxylate | HCID 267210 | — |
| Edukt | Sodium | HCID 5360545 | — |
| Edukt | Tropenol | HCID 53629842 | — |
| Lösungsmittel | Acetonitrile | HCID 6342 | — |
| Produkt | Tropenol 9-hydroxyfluorene-9-carboxylate | HCID 86593872 | — |
Reaktionsschritte
13.4 g (0.056 mol) of methyl ester 3a, 11.65 g (0.084 mol) of tropenol, and 0.3 g of sodium are heated as a melt at 75 mbar for 4 hours over a bath of boiling water with occasional agitation. After cooling, the sodium residues are dissolved with acetonitrile, the solution is evaporated to dryness, and the residue is extracted with dichloromethane/water. The organic phase is washed with water, dried over magnesium sulfate (MgSO4), and the solvent is distilled off. The product is purified by recrystallization from diethyl ether. Yield: 11.40 g of white crystals (29% of theoretical yield).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07429600B2 |
| Quelldatensatz | uspto-grants-2008_09 |
| ORD ID | ord-b304d4c32fef404f97a5da0ed3d58746 |
| Quellennotiz | uspto-grants-2008_09 |