反应详情

According to Scheme 32 Step 1: 2-Methoxy-5-(4-methoxybenzyloxy)pyridine (1.38 mmol, 339 mg), 4-chlorobenzylchloride (2.76 mmol, 468 mg), NaI (1.38 mmol, 207 mg) in acetonitrile (15 mL) was heated at 150° C. for 50 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 CH2Cl2 and CH2Cl2/acetone 90/10) yielding 1-(4-chlorobenzyl)-5-(4-methoxybenzyloxy)pyridine-2(1H)-one (141 mg, 29%).

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.)