反応 #5860

ord-e4e95021117a431db55e0845d2ecf3fd

反応条件

温度
90°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他A three-necked flask equipped with a dropping funnel
  2. 2
    その他While the resultant reaction solution
  3. 3
    その他During the stirring, an exothermic reaction
  4. 4
    その他a large amount of white solid was precipitated
  5. 5
    その他The resultant reaction mixture
  6. 6
    温度cooled
  7. 7
    ろ過filtered
  8. 8
    その他White crystals were obtained in an amount of 58.0 g

実験手順

A three-necked flask equipped with a dropping funnel, a thermometer, and a reflux condenser was charged with 18.6 g of aniline and the aniline was dissolved in 200 ml of toluene. While the resultant reaction solution was stirred with a magnetic stirrer, 42.0 g of toluenesulfonylisocyanate were added dropwise from the dropping funnel to the reaction solution. During the stirring, an exothermic reaction occurred and a large amount of white solid was precipitated. The resultant reaction mixture was heated at a temperature of 90° C. for one hour, cooled, and then filtered. White crystals were obtained in an amount of 58.0 g. The crystals had a melting point of 166° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05246906uspto-grants-1993_09