反应 #65059

ord-80ec530aebed4d97b9df6f3bc2ca43d1

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他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
    其他A clear red solution was obtained
  5. 5
    workup.ADDITIONwas added
  6. 6
    其他to destroy the excess nitrous acid

实验过程

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.

来源

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