반응 #1537

ord-8f3db3635526422b993dd23dd01d5b7e

반응 방정식

CC(=O)OC(CCl)c1ccsc1S(=O)(=O)NC(C)(C)C
N-t-butyl-3-(1-acetoxy-2-chloroethyl)-2-thiophenesulfonamide
CC(=O)OC(CCl)c1ccsc1S(N)(=O)=O
pure title compound
수율 72.0%
CC(=O)OC(CCl)c1ccsc1S(N)(=O)=O
3-(1-acetoxy-2-chloroethyl)-2-thiophenesulfonamide
수율 72.0%

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
    세척the solution was washed with aqueous sodium bicarbanate solution
  4. 4
    기타The organic layer was separated
  5. 5
    건조dried over anhydrous magnesium sulfate
  6. 6
    여과filtered
  7. 7
    농축The filtrate was then concentrated

실험 절차

1.5 g (0.0044 mole) of N-t-butyl-3-(1-acetoxy-2-chloroethyl)-2-thiophenesulfonamide synthesized in Example 7 was 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 the solution was washed with aqueous sodium bicarbanate solution. The organic layer was separated, dried over anhydrous magnesium sulfate and filtered. The filtrate was then concentrated. The residue was subjected to column chromatograpy on silica gel to obtain 760 mg (Yield: 72%) of the pure title compound.

출처

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