Reaktion #65059

Reaktionsgleichung

urea

4-Fluoroaniline

sulphuric acid

sodium nitrite

→

4-Fluorobenzenediazonium hydrogensulphate

Lösungsmittel

water

water

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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.

Quelle