Potassium Carbonate → Pyridine, 2,6-dichloro-4-[1-(trifluoromethyl)ethenyl]-

2,6-dichloro-4-iodopyridine (0.87 g), (3,3,3-trifluoroprop-1-en-2-yl)boronic acid (purity: 65%, 0.75 g) and potassium carbonate (0.96 g) were dissolved in the mixed solvent of THF and water, which was then degassed three times. To the solution was added dichlorobis(triphenylphosphine) palladium (II) (0.04 g), and the mixture was heated to reflux for 3 hours under argon atmosphere. The mixture was cooled to room temperature and then poured into water, which was then extracted twice with hexane. The organic layer was combined, which was then washed with water and dried over anhydrous magnesium sulfate. After the drying agent was filtered off, the solvent was distilled away under reduced pressure, and the residue was then purified by silica gel chromatography to obtain 2,6-dichloro-4-(3,3,3-trifluoroprop-1-en-2-yl)pyridine (0.70 g) at a yield of 82%.

1. customwas then degassed three times
2. additionTo the solution was added dichlorobis(triphenylphosphine) palladium (II) (0.04 g)
3. temperaturethe mixture was heated
4. temperatureto reflux for 3 hours under argon atmosphere
5. additionpoured into water, which
6. extractionwas then extracted twice with hexane
7. washwhich was then washed with water
8. dry with materialdried over anhydrous magnesium sulfate
9. filtrationAfter the drying agent was filtered off
10. distillationthe solvent was distilled away under reduced pressure
11. customthe residue was then purified by silica gel chromatography

ORD 기록

ord-9493ab656e414edcb2590b6e47b85908

출처 데이터셋

uspto-grants-2013_04

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US08410141B2