反应详情

4.80 g (0.02 mol) of methyl 2,2-diphenylpropionate 3b, 2.78 g (0.02 mol) of tropenol, and 0.046 g of sodium are heated as a melt at 75 mbar for 4 hours over a bath of boiling water, shaking from time to time. After cooling, the sodium residues are dissolved with acetonitrile, the solution is evaporated to dryness, and the residue extracted with dichloromethane/water. The organic phase is washed with water, dried over MgSO4, and evaporated to dryness. From the residue, 4c is precipitated as the hydrochloride and this is recrystallized from acetone. Yield: 5.13 g (67% of theory); TLC: Rf value: 0.28 (eluent: sec-butanol/formic acid/water 75:15:10); melting point: 134° C.-135° C.

1. temperatureAfter cooling
2. customthe solution is evaporated to dryness
3. extractionthe residue extracted with dichloromethane/water
4. washThe organic phase is washed with water
5. dry with materialdried over MgSO4
6. customevaporated to dryness
7. customFrom the residue, 4c is precipitated as the hydrochloride
8. customthis is recrystallized from acetone