반응 #59019

ord-887166da898c4f14ba6a5603f09da6c5

반응 방정식

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

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도cooled
  2. 2
    workup.STIRRINGThe mixture was stirred at room temperature for 30 min
  3. 3
    추출The resulting mixture was extracted with ethyl acetate
  4. 4
    세척The organic layer was washed with water and brine
  5. 5
    건조dried over anhydrous magnesium sulfate
  6. 6
    기타The solvent was evaporated under reduced pressure

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07423185B2uspto-grants-2008_09