反応 #59019

ord-887166da898c4f14ba6a5603f09da6c5

反応方程式

Cl
hydrochloric acid
O=S(=O)(OS(=O)(=O)C(F)(F)F)C(F)(F)F
Trifluoromethanesulfonic anhydride
COC(=O)c1ccc(O)cc1OC
methyl 4-hydroxy-2-methoxybenzoate
c1ccncc1
pyridine
COC(=O)c1ccc(OS(=O)(=O)C(F)(F)F)cc1OC
methyl 2-methoxy-4-trifluoromethanesulfonyloxybenzoate

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度cooled
  2. 2
    workup.STIRRINGThe mixture was stirred at room temperature for 30 min
  3. 3
    抽出The resulting mixture was extracted with ethyl acetate
  4. 4
    洗浄The organic layer was washed with water and brine
  5. 5
    乾燥dried over anhydrous magnesium sulfate
  6. 6
    その他The solvent was evaporated under reduced pressure

実験手順

Trifluoromethanesulfonic anhydride (2.24 mL) was added to an ice-cooled mixture of methyl 4-hydroxy-2-methoxybenzoate (2.02 g) and pyridine (0.14 mL) in methylene chloride (15 mL) with stirring. The mixture was stirred at room temperature for 30 min, and poured into a mixture of hydrochloric acid and ethyl acetate. The resulting mixture was extracted with ethyl acetate. The organic layer was washed with water and brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure to afford methyl 2-methoxy-4-trifluoromethanesulfonyloxybenzoate (3.49 g).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07423185B2uspto-grants-2008_09