反应详情

A mixture of 100 g (0.637 mole) of ethyl isonipecotate, 80.64 g (0.64 mole) of benzyl chloride and 67.84 g (0.64 mole) of sodium carbonate in 1 liter of absolute ethanol was heated at reflux for 8 hours and then was stirred at room temperature for 10 hours. The solvent was removed in vacuo, and the residue was partitioned between methylene chloride and dilute sodium hydroxide. The methylene chloride phase was dried over magnesium sulfate and the solvent was removed in vacuo to give the free base of the title compound as a liquid. The free base was converted to the hydrochloric acid salt, and the salt was recrystallized from ethanol-ether to give 89.33 g (49.7%) of white, crystalline solid, m.p. 154°-155° C.

1. temperaturewas heated
2. temperatureat reflux for 8 hours
3. customThe solvent was removed in vacuo
4. customthe residue was partitioned between methylene chloride and dilute sodium hydroxide
5. dry with materialThe methylene chloride phase was dried over magnesium sulfate
6. customthe solvent was removed in vacuo