反応 #2460321

ord-7f446ff3ec824f87ab856c6400036cd9

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.STIRRINGThe reaction mixture was stirred overnight at room temperature
  2. 2
    抽出extracted three times with ether (3×100 ml )
  3. 3
    洗浄The combined organic layer was washed with saturated sodium chloride solution
  4. 4
    乾燥dried over anhydrous magnesium sulfate
  5. 5
    その他After removal of solvent
  6. 6
    workup.DISTILLATIONthe product was purified by distillation at 117-119° C. (0.5 mmHg)
  7. 7
    その他was isolated in 88.4% (5.72 g)
  8. 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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07459106B2uspto-grants-2008_12