반응 #65059

ord-80ec530aebed4d97b9df6f3bc2ca43d1

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타A smooth paste was formed
  2. 2
    온도The mixture was cooled to <5°
  3. 3
    온도while maintaining the temperature at <5° with external cooling
  4. 4
    기타A clear red solution was obtained
  5. 5
    workup.ADDITIONwas added
  6. 6
    기타to destroy the excess nitrous acid

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05416235uspto-grants-1995_05