반응 #1563890

ord-6f8ebbac375646b1b282f1ad582046b0

반응 방정식

COc1ccccc1NC(=O)c1c(N)cccc1Sc1ccc([N+](=O)[O-])cc1
Compound 25
COc1ccccc1NC(=O)c1c(N)cccc1Sc1ccc([N+](=O)[O-])cc1
2-amino-N-(2-methoxyphenyl)-6-(4-nitrophenylthi-o)benzamide
O=S(=O)(Cl)c1ccccc1
benzenesulfonyl chloride
COc1ccccc1NC(=O)c1c(NS(=O)(=O)c2ccccc2)cccc1Sc1ccc([N+](=O)[O-])cc1
N-(2-methoxyphenyl)-2-(4-nitrophenylthio)-6-(phenylsulfonamido)benzamide
수율 67.0%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축the reaction mixture was concentrated under reduced pressure
  2. 2
    세척washed with water (3×20 mL)
  3. 3
    건조dried over anhydrous Na2SO4
  4. 4
    여과filtered
  5. 5
    농축concentrated under reduced pressure
  6. 6
    기타The residue was purified by silica gel column chromatography (1:4 v/v ethyl acetate/petroleum ether)
  7. 7
    기타to provide a white solid

실험 절차

Compound 25 (1.0 equiv.) was dissolved in azabenzene (40 mL) at room temperature. To this mixture was added benzenesulfonyl chloride (1.2 equiv.). After being stirred for 10 Hours at room temperature, the reaction mixture was concentrated under reduced pressure. The crude residue was diluted ethyl acetate (50 mL), washed with water (3×20 mL), dried over anhydrous Na2SO4, filtered, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (1:4 v/v ethyl acetate/petroleum ether) to provide a white solid. 67% yield;

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09402819B2uspto-grants-2016_08