反应详情

1.50 g (13.8 mmol) of 2-hydroxy-3-methylpyridine in 70 ml of DMF are admixed at 0° C. with 2.31 g (20.6 mmol) of potassium tert-butoxide, and the mixture is stirred at room temperature for 30 min. 2.87 g (15.1 mmol) of 2-chloro-4-fluoro-5-methylnitrobenzene are added while continuing to stir at RT. After 17 h, the mixture is admixed with 1000 ml of water and then extracted three times with ethyl acetate. The combined organic phases are dried over sodium sulfate and, after filtration, the solvents are removed under reduced pressure. The residue is purified by chromatography on silica gel (2:1 cyclohexane/ethyl acetate). This affords 2.15 g (56% of theory) of the desired compound.

1. stirringto stir at RT
2. waitAfter 17 h
3. extractionextracted three times with ethyl acetate
4. dry with materialThe combined organic phases are dried over sodium sulfate
5. filtrationafter filtration
6. customthe solvents are removed under reduced pressure
7. customThe residue is purified by chromatography on silica gel (2:1 cyclohexane/ethyl acetate)