Реакция #1533

ord-79a672ca3eff441b932b12489c10964b

Уравнение реакции

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
Выход 74.0%
CC(=O)OC(CF)c1ccsc1S(N)(=O)=O
3-(1-acetoxy-2-fluoroethyl)-2-thiophenesulfonamide
Выход 74.0%

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Концентрированиеconcentrated under reduced pressure
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in methylene chloride
  3. 3
    Промывкаwashed with aqueous sodium bicarbonate solution
  4. 4
    ДругоеThe organic layer was separated
  5. 5
    Сушкаdried over anhydrous magnesium sulfate
  6. 6
    Фильтрацияfiltered
  7. 7
    КонцентрированиеThe filtrate was concentrated
  8. 8
    ДругоеThe residue was recrystallized

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05726127uspto-grants-1998_03