反应详情

To a solution of 2-amino-6-piperidinobenzonitrile (8.8 g) in methylene chloride (100 ml) is added pyridine (3.3 ml), and thereto is added dropwise acetoxyacetyl chloride (4.3 ml) which is cooled in an ice bath. The mixture is stirred at room temperature for 1 hour, and thereafter, water is added thereto, and the mixture is extracted with methylene chloride. The organic layer is dried over anhydrous sodium sulfate, and the solvent is distilled off under reduced pressure. The resulting crude crystals are recrystallized from ethyl acetate-hexane to give the title compound (3.2 g) having the following physical properties.

1. temperatureis cooled in an ice bath
2. extractionthe mixture is extracted with methylene chloride
3. dry with materialThe organic layer is dried over anhydrous sodium sulfate
4. distillationthe solvent is distilled off under reduced pressure
5. customThe resulting crude crystals are recrystallized from ethyl acetate-hexane