反应详情

To an ice cold solution of isonipecotic acid (90 g, 0.697 mol) and potassium carbonate (81 g, 1.31 mol) in water (1.3 liter) was added dropwise benzoyl chloride (81 ml, 0.697 mol) over a period of about an hour at about 5° C. The mixture was stirred at room temperature overnight. The reaction mixture was acidified with 6N hydrochloric acid and extracted with dichloromethane. The organic layer was washed with water and then dried over magnesium sulfate and the solvent was evaporated in vacuo. Crystallization from isopropyl alcohol-diethyl ether to give the titled compound (154.4 g).

1. extractionextracted with dichloromethane
2. washThe organic layer was washed with water
3. dry with materialdried over magnesium sulfate
4. customthe solvent was evaporated in vacuo
5. customCrystallization from isopropyl alcohol-diethyl ether