Reaktion #4335

Reaktionsgleichung

4,5-dichloro-2-nitro-N-β-aminoethylaniline

monoethanolamine

→

2-chloro-5-β-aminoethylamino-4-nitro-N-(β-hydroxyethyl)aniline

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeAn impurity is precipitated
2. 2
   workup.ADDITIONby adding hydrochloric acid
3. 3
   Sonstigeis removed by filtration
4. 4
   SonstigeThe expected product precipitates
5. 5
   FiltrationAfter filtration
6. 6
   Sonstigedrying
7. 7
   Sonstigeit is purified as its hydrochloride
8. 8
   Sonstigebefore being recrystallized from alcohol

Vorschrift

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.

Quelle