Реакция #65059

ord-80ec530aebed4d97b9df6f3bc2ca43d1

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

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

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05416235uspto-grants-1995_05