反应详情

To a round bottom flask (500 mL) equipped with a magnetic stirrer and condenser were added 2.0 g (9.0 mmol) of 5-tert-butyl-2-methyl-4-thiocyanato-phenol (prepared in Example GGG), cesium carbonate (5.88 g, 18.0 mmol), sodium iodide (4.8 g, 32.0 mmol), and acetonitrile (100 mL). This suspension was heated to reflux for 30 minutes and bromomethyl acetate (1.76 mL, 18.0 mmol) was added via syringe. The reaction was refluxed overnight, cooled to room temperature, quenched with H2O and extracted with EtOAc. The organic layers were combined and dried (MgSO4). The solvent was evaporated and the residue dried under high vacuum to give the title compound. 1H NMR (CDCl3) δ 1.46 (s, 9 H), 2.26 (s, 3 H), 3.82 (s, 3 H), 4.68 (s, 2 H), 6.69 (s, 1 H), 7.52 (s, 1 H),

1. customTo a round bottom flask (500 mL) equipped with a magnetic stirrer and condenser
2. temperatureThis suspension was heated
3. temperatureto reflux for 30 minutes
4. temperatureThe reaction was refluxed overnight
5. customquenched with H2O
6. extractionextracted with EtOAc
7. dry with materialdried (MgSO4)
8. customThe solvent was evaporated
9. customthe residue dried under high vacuum