反应详情

According to Scheme 32 Step 1: 5-(4-Fluorophenoxy)-2-methoxypyridine (2.37 mmol, 520 mg), 4-chlorobenzylchloride (3.55 mmol, 603 mg), NaI (2.37 mmol, 356 mg) in acetonitrile (15 mL) was heated at 150° C. for 20 minutes under microwave conditions. The cooled crude reaction washed with water, extracted with AcOEt. The organic layer was collected, dried (Na2SO4) and the solvent was evaporated under reduced pressure. The residue was purified in a manifold (vac.) using a Sep-Pak silica cartridge (heptane/AcOEt, 90:10 to CH2Cl2) and then CH2Cl2/acetone 90:10), following HPLC purification yielding 1-(4-chlorobenzyl)-5-(4-fluorophenoxy)pyridin-2(1H)-one (211 mg, 27%).

1. temperatureThe cooled crude
2. customreaction
3. washwashed with water
4. extractionextracted with AcOEt
5. customThe organic layer was collected
6. dry with materialdried (Na2SO4)
7. customthe solvent was evaporated under reduced pressure
8. customThe residue was purified in a manifold (vac.)
9. customHPLC purification