反应详情

A mixture of 5-(4-methoxyphenyl)-1-((6-(2-(trimethylsilyl)ethynyl)pyridin-3-yl)methyl)pyridin-2(1H)-one (0.60 mmol, 240 mg), tetrabutylammonium fluoride (1.20 mmol, 1.2 mL) in THF (5 mL) and H2O (1 mL) was stirred at room temperature for 2 hours. The solvent was evaporated under reduced pressure. The residue was taken up in CH2Cl2, washed with water, dried (Na2SO4) and evaporated under reduced pressure. The residue was purified in a manifold (vac.) using a Sep-Pak silica cartridge CH2Cl2/MeOH(NH3)sat. 3%. The fractions were collected and evaporated. The residue thus obtained was triturated with diisopropyl ether. The precipitated solid was filtered off and dried. Further purification by circular chromatography-TLC CH2Cl2/MeOH(NH3)sat. 3% yielding 1-((6-ethynylpyridin-3-yl)methyl)-5-(4-methoxyphenyl)pyridin-2(1H)-one (68 mg, 35%).

1. customThe solvent was evaporated under reduced pressure
2. washwashed with water
3. dry with materialdried (Na2SO4)
4. customevaporated under reduced pressure
5. customThe residue was purified in a manifold (vac.)
6. customThe fractions were collected
7. customevaporated
8. customThe residue thus obtained
9. customwas triturated with diisopropyl ether
10. filtrationThe precipitated solid was filtered off
11. customdried
12. customFurther purification by circular chromatography-TLC CH2Cl2/MeOH(NH3)sat