반응 #1533

ord-79a672ca3eff441b932b12489c10964b

반응 방정식

CC(=O)OC(CF)c1ccsc1S(=O)(=O)NC(C)(C)C
N-t-butyl-3-(1-aceoxy-2-fluoroethyl) 2-thiophenesulfonamide
CC(=O)OC(CF)c1ccsc1S(=O)(=O)NC(C)(C)C
N-t-butyl-3-(1-acetoxy-2-fluoroethyl)-2-thiophenesulfonamide
CC(=O)OC(CF)c1ccsc1S(N)(=O)=O
pure title compound
수율 74.0%
CC(=O)OC(CF)c1ccsc1S(N)(=O)=O
3-(1-acetoxy-2-fluoroethyl)-2-thiophenesulfonamide
수율 74.0%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축concentrated under reduced pressure
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in methylene chloride
  3. 3
    세척washed with aqueous sodium bicarbonate solution
  4. 4
    기타The organic layer was separated
  5. 5
    건조dried over anhydrous magnesium sulfate
  6. 6
    여과filtered
  7. 7
    농축The filtrate was concentrated
  8. 8
    기타The residue was recrystallized

실험 절차

1.4 g (0.0043 mole) of N-t-butyl-3-(1-aceoxy-2-fluoroethyl) -2-thiophenesulfonamide synthesized in Example 2 dissolved in 5 ml of trifluoroacetic acid. The reaction solution was stirred at normal temperature for 12 hours and then concentrated under reduced pressure. The residue was dissolved in methylene chloride and washed with aqueous sodium bicarbonate solution. The organic layer was separated, dried over anhydrous magnesium sulfate and then filtered. The filtrate was concentrated. The residue was recrystallized to obtain 750 mg (Yield: 74%) of the pure title compound as a white solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05726127uspto-grants-1998_03