反応 #1563890

ord-6f8ebbac375646b1b282f1ad582046b0

反応方程式

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
収率 67.0%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮the reaction mixture was concentrated under reduced pressure
  2. 2
    洗浄washed with water (3×20 mL)
  3. 3
    乾燥dried over anhydrous Na2SO4
  4. 4
    ろ過filtered
  5. 5
    濃縮concentrated under reduced pressure
  6. 6
    その他The residue was purified by silica gel column chromatography (1:4 v/v ethyl acetate/petroleum ether)
  7. 7
    その他to provide a white solid

実験手順

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;

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09402819B2uspto-grants-2016_08