反应详情

2-Amino-6-chlorobenzoic acid (25.0 g, 143 mmol) was dissolved in 120 mL of anhydrous THF in a 500 mL 2 neck round bottom flask. The solution was cooled in an ice-water bath. 215 mL of 1.0 M lithium aluminum hydride (LAH) THF solution was then added dropwise. After all of the LAH was added, the reaction mixture was allowed to warm up to room temperature and then stirred at room temperature overnight. ˜10 mL of water was added to the reaction mixture followed by 7 g 15% NaOH. An additional 20 g of water was added to the reaction mixture. The organic THF phase was decanted and ˜200 mL of ethyl acetate was added to the solid with stirring. Na2SO4 was added as a drying agent to the combined ethyl acetate organic portion and THF portion. The mixture was filtered and evaporated. ˜20 g yellow solid was obtained and taken on to the next step without further purification.

1. temperatureThe solution was cooled in an ice-water bath
2. customThe organic THF phase was decanted
3. addition˜200 mL of ethyl acetate was added to the solid
4. stirringwith stirring
5. additionNa2SO4 was added as a drying agent to the combined ethyl acetate organic portion and THF portion
6. filtrationThe mixture was filtered
7. customevaporated