反应详情

To a suspension of 3-fluoropicolinic acid (17.7 g) in THF (300 mL) was added CDI (22.4 g) at room temperature, and the mixture was stirred at room temperature for 30 min and heated to 50° C. After stirring at 50° C. for 1 h, the mixture was cooled to room temperature. To the mixture were added N,O-dimethylhydroxylamine hydrochloride (18.4 g) and DIPEA (32.9 mL) at room temperature, and the mixture was stirred at room temperature for 12 h. The mixture was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (AcOEt) to give the title compound (21.8 g).

1. temperatureheated to 50° C
2. stirringAfter stirring at 50° C. for 1 h
3. temperaturethe mixture was cooled to room temperature
4. stirringthe mixture was stirred at room temperature for 12 h
5. concentrationThe mixture was concentrated under reduced pressure
6. customThe residue was purified by silica gel column chromatography (AcOEt)