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2, 4, 4'-trinitrobenzene formanilide preparation method

A technology of trinitrobenzanilide and nitrobenzoyl chloride, which is applied in the field of preparation of 2,4,4'-trinitrobenzanilide, and can solve the problems of large environmental pollution, low yield and great discomfort Problems such as large-scale production, to achieve the effect of environmental protection and increase yield

Active Publication Date: 2014-05-07
大连新阳光材料科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the preparation method of 2,4,4'-trinitrobenzanilide needs to be carried out in the presence of a solvent on the one hand, so that the environmental pollution is relatively large, on the other hand, the yield is also low, and it is not suitable for large-scale industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1）

[0009] The preparation method of 2,4,4'-trinitrobenzanilide of the present embodiment has the following steps:

[0010] ①In a nitrogen atmosphere, add 18.3g of 2,4-dinitroaniline (0.1mol) and 24.1g of p-nitrobenzoyl chloride (0.13mol) into the reaction device, stir and heat up to 180°C for 12h .

[0011] ②After the reaction, the temperature was raised to 198°C, and the unreacted p-nitrobenzoyl chloride was recovered by distillation.

[0012] ③ Then, the temperature was lowered to 145°C, and under a pressure of 15 mmHg, 32.0 g of 2,4,4'-trinitrobenzanilide was obtained by distillation under reduced pressure, with a yield of 96.4%.

Embodiment 2）

[0014] The preparation method of 2,4,4'-trinitrobenzanilide of the present embodiment has the following steps:

[0015] ①In a nitrogen atmosphere, add 18.3g of 2,4-dinitroaniline (0.1mol) and 27.8g of p-nitrobenzoyl chloride (0.15mol) into the reaction device, stir and heat up to 185°C for 10h .

[0016] ②After the reaction, the temperature was raised to 200°C, and the unreacted p-nitrobenzoyl chloride was recovered by distillation.

[0017] ③Then, the temperature was lowered to 150°C, and under a pressure of 10mmHg, 31.8g of 2,4,4'-trinitrobenzanilide was obtained by distillation under reduced pressure, with a yield of 95.8%.

Embodiment 3）

[0019] The preparation method of 2,4,4'-trinitrobenzanilide of the present embodiment has the following steps:

[0020] ①In a nitrogen atmosphere, add 18.3g g of 2,4-dinitroaniline (0.1mol) and 20.4g of p-nitrobenzoyl chloride (0.11mol) into the reaction device, stir and heat up to 178°C for 15h .

[0021] ②After the reaction, the temperature was raised to 195°C, and the unreacted p-nitrobenzoyl chloride was recovered by distillation.

[0022] ③Then, the temperature was lowered to 140°C, and under a pressure of 20mmHg, 31.3g of 2,4,4'-trinitrobenzanilide was obtained by vacuum distillation, with a yield of 94.3%.

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PUM

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Abstract

The invention discloses a 2, 4, 4'-trinitrobenzene formanilide preparation method, which includes the steps: firstly, adding 2, 4-dinitroaniline and paranitrobenzoyl chloride into a reaction device in a nitrogen atmosphere, stirring and increasing the temperature to 178-185 DEG C for reaction of 10h-15h, wherein the molar ratio of the 2, 4-dinitroaniline to paranitrobenzoyl chloride is 1:1.1-1:1.5; secondly, increasing the temperature to 195-200 DEG C, and distilling to recover unreacted paranitrobenzoyl chloride; and thirdly, cooling to 140-150 DEG C, so that 2, 4, 4'-trinitrobenzene formanilide is obtained by means of reduced pressure distillation. By the method, the reaction temperature can be controlled to be higher than the melting points of the two kinds of raw materials, so that condensation reaction can be performed in the molten state, solvent is not needed, environmental protection is benefited, yield is greatly increased, and the method is suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and in particular relates to a preparation method of 2,4,4'-trinitrobenzanilide. Background technique [0002] 2,4,4'-Trinitrobenzanilide is an important chemical intermediate, and the 2,4,4'-triaminobenzanilide obtained by its catalytic hydrogenation can be further cyclized to obtain synthetic aramid fibers An important monomer of aminobenzimidazole derivatives. [0003] At present, the preparation method of 2,4,4'-trinitrobenzanilide needs to be carried out in the presence of a solvent on the one hand, so that the environmental pollution is relatively large, on the other hand, the yield is also low, and it is not suitable for large-scale industrial production . Contents of the invention [0004] The object of the present invention is to solve the above problems, and to provide a method for preparing 2,4,4'-trinitrobenzanilide without solvent and with high yield. [0005] The technical solutio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C233/66C07C231/02
Inventor 胡国宜胡雪明周国平游劲松兰静波
Owner 大连新阳光材料科技有限公司
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