反应详情

13.65 g (0.053 mol) of methylester 3a, 8.35 g (0.06 mol) of tropenol and 0.2 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. Then the organic phase is washed with water, dried over magnesium sulfate, and the solvent is distilled off. The product is purified by recrystallization from diethyl ether/petroleum ether. Yield: 5.28 g of white crystals (27% of theoretical yield); melting point: 117° C.

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