反应详情

Methyl 6-chloro-5-fluoropicolinate (1.35 g, 7.095 mmol) was dissolved in THF:H2O=6:1 (42 ml), followed by addition of lithium hydroxide monohydrate (596 mg, 14.19 mmol), and then the resulting mixture was stirred at room temperature for 3 hours. The resulting reaction liquid was concentrated under reduced pressure, dissolved by addition of distilled water (20 ml), acidified by slow addition of 1N aqueous HCl solution, and then extracted with 5% MeOH/MC (30 ml×2). The organic layer was dried over anhydrous sodium sulfate, followed by filtration, concentration, and vacuum drying, to obtain 1.04 g of white solid (80%).

1. customThe resulting reaction liquid
2. concentrationwas concentrated under reduced pressure
3. dissolutiondissolved by addition of distilled water (20 ml)
4. additionacidified by slow addition of 1N aqueous HCl solution
5. extractionextracted with 5% MeOH/MC (30 ml×2)
6. dry with materialThe organic layer was dried over anhydrous sodium sulfate
7. filtrationfollowed by filtration, concentration, and vacuum
8. customdrying