反应详情

To 5 ml of pyridine was dissolved 0.62 g (2.3 mmol) of 6,6-difluoro-5-methyl-5-hexenyl 6-aminonicotinate, followed by the addition of 0.48 g (2.5 mmol) of toluene-4-sulfonylchloride under ice-cooling, stirring for 10 minutes and then stirring at room temperature for 15 hours. The reaction liquid was then poured in 5% hydrochloric acid and extracted with ethyl acetate. The organic layer was washed with water and a saturated saline solution in this order, followed by drying over anhydrous magnesium sulfate and concentration under reduced pressure. The residue was purified with silica gel column chromatography (ethyl acetate:hexane=1:2) to obtain 0.88 g (yield: 90%) of 6,6-difluoro-5-methyl-5-hexenyl 6-(toluene-4-sulfonylamino)nicotinate.

1. temperaturecooling
2. stirringstirring at room temperature for 15 hours
3. customThe reaction liquid
4. extractionextracted with ethyl acetate
5. washThe organic layer was washed with water
6. dry with materialby drying over anhydrous magnesium sulfate and concentration under reduced pressure
7. customThe residue was purified with silica gel column chromatography (ethyl acetate:hexane=1:2)