反応 #65059

ord-80ec530aebed4d97b9df6f3bc2ca43d1

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他A smooth paste was formed
  2. 2
    温度The mixture was cooled to <5°
  3. 3
    温度while maintaining the temperature at <5° with external cooling
  4. 4
    その他A clear red solution was obtained
  5. 5
    workup.ADDITIONwas added
  6. 6
    その他to destroy the excess nitrous acid

実験手順

4-Fluoroaniline (11.2 g; 0.1 mol) was added dropwise into a solution of sulphuric acid (25 g) in water (60 ml) over 10 min. A smooth paste was formed. The mixture was cooled to <5° and a solution of sodium nitrite (7.8 g; 0.11 mol) in water (25 ml) was added dropwise over 0.5 hours while maintaining the temperature at <5° with external cooling. A clear red solution was obtained. The solution was stirred for 0.25 hours to complete the reaction and urea (1.0 g) was added to destroy the excess nitrous acid. The resulting solution was used directly in the next stage.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05416235uspto-grants-1995_05