反応 #2460321
ord-7f446ff3ec824f87ab856c6400036cd9
反応条件
後処理
- 1workup.STIRRINGThe reaction mixture was stirred overnight at room temperature
- 2抽出extracted three times with ether (3×100 ml )
- 3洗浄The combined organic layer was washed with saturated sodium chloride solution
- 4乾燥dried over anhydrous magnesium sulfate
- 5その他After removal of solvent
- 6workup.DISTILLATIONthe product was purified by distillation at 117-119° C. (0.5 mmHg)
- 7その他was isolated in 88.4% (5.72 g)
- 8その他yield
実験手順
4-Bromobenzenethiol (5 g, 26.44 mmol) was added to a solution of sodium methoxide (1.43 g, 26.48 mmol) in 20 ml of anhydrous methanol. The mixture was stirred for 30 min under nitrogen at room temperature and a solution of methyl iodide (4.51 g, 31.77 mmol) in 20 ml anhydrous methanol was then added. The reaction mixture was stirred overnight at room temperature, poured into 2 M of NaOH aqueous solution (30 ml) and extracted three times with ether (3×100 ml ). The combined organic layer was washed with saturated sodium chloride solution and dried over anhydrous magnesium sulfate. After removal of solvent, the product was purified by distillation at 117-119° C. (0.5 mmHg) and was isolated in 88.4% (5.72 g) yield.