反应详情

5-trimethylsilylethynyl-3-(1-(2,6-dichloro-3-fluorophenyl)ethoxy)-2-aminopyridine (1.5 g, 3.77 mmol) was dissolved in the mixed solvent of THF (10 mL) and MeOH (10 mL), K2CO3 (1.04 g, 7.55 mmol) was added, and the mixture was stirred for 2 h at room temperature. The majority of the solvent was removed under reduced pressure, water (10 mL) was added. The resultant mixture was extracted with ethyl acetate (3×20 mL), the organic phases were combined, washed with water and saturated brine successively, dried over anhydrous sodium sulfate, and then concentrated, the resultant residue was purified via silica gel column chromatography (petroleum ether/ethyl acetate=3:1) to yield 850 mg of the target product as brown solid.

1. additionwas added
2. customThe majority of the solvent was removed under reduced pressure, water (10 mL)
3. additionwas added
4. extractionThe resultant mixture was extracted with ethyl acetate (3×20 mL)
5. washwashed with water and saturated brine successively
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationconcentrated
8. customthe resultant residue was purified via silica gel column chromatography (petroleum ether/ethyl acetate=3:1)