HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → Tropenol 9-hydroxyfluorene-9-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl 9-hydroxy-9H-fluorene-9-carboxylate | HCID 267210 | — |
| Reactant | Sodium | HCID 5360545 | — |
| Reactant | Tropenol | HCID 53629842 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | Tropenol 9-hydroxyfluorene-9-carboxylate | HCID 86593872 | — |
Reaction Steps
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).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07214797B2 |
| Source dataset | uspto-grants-2007_05 |
| ORD ID | ord-1497911858224227891bdc8a08228a86 |
| Source note | uspto-grants-2007_05 |