反応 #65059
ord-80ec530aebed4d97b9df6f3bc2ca43d1
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1その他A smooth paste was formed
- 2温度The mixture was cooled to <5°
- 3温度while maintaining the temperature at <5° with external cooling
- 4その他A clear red solution was obtained
- 5workup.ADDITIONwas added
- 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.