Reaktion #2061804

Reaktionsgleichung

1-Chloro-2,5-difluoro-4-nitrobenzene

diethylamine

cyclopropylamine

→

5-chloro-N-cyclopropyl-4-fluoro-2-nitroaniline

Ausbeute 79.9%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeAfter 1 hour at 0° the suspension obtained
2. 2
   Extraktionextracted with ethyl acetate
3. 3
   WaschenThe organic phase is washed with 10 percent sodium chloride solution
4. 4
   Trocknendried over magnesium sulfate
5. 5
   workup.DISTILLATIONAfter distillation of the solvent the residue
6. 6
   Sonstigeis recrystallized from ethanol (50 ml)

Vorschrift

1-Chloro-2,5-difluoro-4-nitrobenzene (3.69 g, 19 mmol) is treated at 0° with diethylamine (2.3 g, 23 mmol) and cyclopropylamine (1.3 g, 23 mmol). After 1 hour at 0° the suspension obtained is stirred at 25° for 16 hours. The reaction mixture is taken up in water (150 ml) and extracted with ethyl acetate. The organic phase is washed with 10 percent sodium chloride solution and dried over magnesium sulfate. After distillation of the solvent the residue is recrystallized from ethanol (50 ml). There are obtained 3.5 g (79%) of 5-chloro-N-cyclopropyl-4-fluoro-2-nitroaniline with a m.p. of 73.5°-75.5°.

Quelle