반응 #62532

반응 방정식

2,4-dinitroaniline

triethylamine

3,5-dinitrobenzoyl chloride

→

2',3,4',5-tetranitrobenzanilide

수율 8.1%

용매

benzene

반응 조건

후처리

1. 1
   온도refluxed
2. 2
   온도under heating for 6 hours
3. 3
   여과The reaction mixture was filtered in hot state
4. 4
   온도the filtrate was cooled
5. 5
   여과was collected by filtration

실험 절차

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.

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