反応 #4335
ord-4c54e3751d4842d7a5094d5ea6aa2e59
反応方程式
4,5-dichloro-2-nitro-N-β-aminoethylaniline
monoethanolamine
→
2-chloro-5-β-aminoethylamino-4-nitro-N-(β-hydroxyethyl)aniline
溶媒
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1その他An impurity is precipitated
- 2workup.ADDITIONby adding hydrochloric acid
- 3その他is removed by filtration
- 4その他The expected product precipitates
- 5ろ過After filtration
- 6その他drying
- 7その他it is purified as its hydrochloride
- 8その他before being recrystallized from alcohol
実験手順
0.04 mole (10 g) of 4,5-dichloro-2-nitro-N-β-aminoethylaniline prepared in the 1st stage is heated in 40 ml of monoethanolamine for 30 minutes to 100° C. The reaction mixture is diluted with 450 ml of iced water. An impurity is precipitated by adding hydrochloric acid and is removed by filtration. The filtrate is made alkaline with concentrated sodium hydroxide solution. The expected product precipitates. After filtration and drying, it is purified as its hydrochloride before being recrystallized from alcohol. It melts at 160° C.