反应 #1563890

ord-6f8ebbac375646b1b282f1ad582046b0

反应方程式

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
收率 67.0%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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;

来源

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