反应详情

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).

1. temperatureAfter cooling
2. customthe solution is evaporated to dryness
3. extractionthe residue is extracted with dichloromethane/water
4. washThe organic phase is washed with water
5. dry with materialdried over magnesium sulfate (MgSO4)
6. distillationthe solvent is distilled off
7. customThe product is purified by recrystallization from diethyl ether