Reaktion #62532

Reaktionsgleichung

2,4-dinitroaniline

triethylamine

3,5-dinitrobenzoyl chloride

→

2',3,4',5-tetranitrobenzanilide

Ausbeute 8.1%

Lösungsmittel

benzene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturrefluxed
2. 2
   Temperaturunder heating for 6 hours
3. 3
   FiltrationThe reaction mixture was filtered in hot state
4. 4
   Temperaturthe filtrate was cooled
5. 5
   Filtrationwas collected by filtration

Vorschrift

2,4-dinitroaniline (18.05 g), triethylamine (12.97 g) and benzene (750 ml) were placed in a reaction vessel and stirred under the nitrogen atmosphere. To the reaction mixture, 3,5-dinitrobenzoyl chloride (25.00 g) was added and refluxed under heating for 6 hours. The reaction mixture was filtered in hot state and the filtrate was cooled to deposit crystals of 2',3,4',5-tetranitrobenzanilide which was collected by filtration. The product of 2',3,4',5-tetranitrobenzanilide (3.00 g) thus obtained, platinum/carbon (5%) (0.18 g) and dioxane (85 ml) were placed in a pressurized vessel and allowed to react under the hydrogen pressure of 1 to 3 kg/cm2 at 80° C. for 10 hours. After cooling, the catalyst was removed by filtration and dioxane was distilled off under the reduced pressure to obtain powder of 2',3,4',5-tetraaminobenzanilide.

Quelle