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Preparation method of 1, 5-dichloro-2, 4-dinitrobenzene

A technology of dinitrobenzene and dinitrobenzene, which is applied in the field of compound preparation, can solve the problems of a large amount of waste acid environment, pollution, and high reaction temperature, and achieve the effect of low requirements for reaction equipment, abundant raw material sources, and high purity

Pending Publication Date: 2021-07-09
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But this kind of method has high reaction temperature and fuming nitric acid-concentrated sulfuric acid will produce a large amount of nitrogen oxide gas and too much waste acid and cause environmental pollution

Method used

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  • Preparation method of 1, 5-dichloro-2, 4-dinitrobenzene
  • Preparation method of 1, 5-dichloro-2, 4-dinitrobenzene
  • Preparation method of 1, 5-dichloro-2, 4-dinitrobenzene

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Embodiment 1

[0015] The embodiment of the present invention provides a preparation method of 1,5-dichloro-2,4-dinitrobenzene, using m-dichlorobenzene as raw material, N-nitropyrazole and H 2 SO 4 For the preparation of 1,5-dichloro-2,4-dinitrobenzene as a nitrating agent, the synthetic route is as follows figure 1 Shown; specifically include the following steps: take 8ml of 98% sulfuric acid in a four-necked flask, add m-dichlorobenzene 0.012mol dropwise to the concentrated sulfuric acid under mechanical stirring (300-400 rpm) at 20°C, and complete the addition in a water bath Raise the temperature to 60°C, add 0.024mol of N-nitropyrazole in batches at this temperature (the reaction system will heat up during the feeding process, and add again after the temperature drops to the initial temperature), keep stirring after the feeding is completed, and react at a constant temperature of 65°C 6h, while hot, pour the reaction solution into a container with ice cubes and stir to reduce the tempe...

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Abstract

The invention discloses a preparation method of 1, 5-dichloro-2, 4-dinitrobenzene. The preparation method comprises the following steps: preparing 1, 5-dichloro-2, 4-dinitrobenzene by using m-dichlorobenzene as a raw material and N-nitropyrazole and H2SO4 as nitrating agents; the method specifically comprises the following steps: adding 8ml of 98% sulfuric acid into a four-neck bottle, dropwise adding 0.012 mol of m-dichlorobenzene into concentrated sulfuric acid under the conditions of mechanical stirring and the temperature of 20 DEG C, heating in a water bath to 60 DEG C after charging is completed, averagely dividing 0.024 mol of N-nitropyrazole into four parts, sequentially adding the four parts of N-nitropyrazole at the temperature, heating the reaction system in the adding process, adding materials again after the temperature is reduced to the initial temperature, keeping stirring after the materials are added, reacting at the constant temperature of 65 DEG C for 6 hours, pouring reaction liquid into a container filled with ice blocks while the reaction liquid is hot, and stirring to reduce the temperature of the solution to 5 DEG C to precipitate suspended solids.

Description

technical field [0001] The invention relates to the field of compound preparation, in particular to a preparation method of 1,5-dichloro-2,4-dinitrobenzene. Background technique [0002] 1,5-dichloro-2,4-dinitrobenzene is mainly used as an intermediate in organic synthesis, and is also used in adjuvants, pesticides, and medicine. 1,5-dichloro-2,4-dinitrobenzene plays an important role in organic synthesis, and its market has always been optimistic. The development of this kind of product has good economic and social benefits. [0003] At present, the preparation of 1,5-dichloro-2,4-dinitrobenzene is obtained by high-temperature nitration of m-dichlorobenzene in a nitric acid mixed acid nitration system. As described in US005574188A, use oleum-nitric acid system to nitrate 1,3-dichlorobenzene, the yield is 89.8%; Li Peng (Li Peng. Preparation of herbicide RH1658 intermediate [D]. Shenyang University of Technology, 2007.) in its In the master's thesis, 59.5g m-dichlorobenzen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/12C07C201/08
CPCC07C201/08C07C205/12
Inventor 李永祥马忠平梁栋赵林秀王艳红胡志勇李军任福德陈芳陈丽珍刘永政张桐伟刘文东刘明张帅郑入水霍媛媛
Owner ZHONGBEI UNIV
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