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A technology of nitrobenzaldehyde and a synthesis method, which is applied in the synthesis field of m-nitrobenzaldehyde, can solve the problems of long process steps, large environmental pollution and high production cost, and achieves low cost of raw materials, simplified steps and short production cycle. Effect
Active Publication Date: 2016-07-20
YUEYANG YETOP FINE CHEM
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Although this method has a very high yield, it also has the following disadvantages: the process steps are long, the production cost is very high, and the amount of waste water produced is very large, and there is also a large amount of nitrate and sulfite in the waste water, which is harmful to the environment. Very big
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Embodiment 1
[0026] A method for synthesizing m-nitrobenzaldehyde, the raw materials and instruments used are shown in Table 1.
[0027] Table 1 Statistics of raw materials and instruments
[0028] Raw materials\parameters
Manufacturer
Specification
Content
Copper nitrate
Unlimited
Second grade
≥99.5%
Silver nitrate
Unlimited
Second grade
≥99.0%
Benzaldehyde
Unlimited
Qualified product
≥99.0%
Reaction device
Unlimited
Three-necked flask
-
[0029] The synthesis of m-nitrobenzaldehyde in this embodiment specifically includes the following steps:
[0030] Step 1: Reaction, specifically: add 19.70 grams (0.105mol) of copper nitrate into the reaction device, slowly add 50 grams (2.78mol) of water at room temperature to completely dissolve the copper nitrate to obtain a copper nitrate solution (here, add water The rate is adjustable, and the purpose is to achieve complete dissolution of copper nitrate); add 0.017 grams (0.000101mol) of silver nitrate to the copper nitrate s...
Embodiment 2- Embodiment 6
[0045] Example 2-Example 6 differs from Example 1 in Table 2.
[0046] Table 2 Example 2-Example 6 Parameter Statistics Table
[0047]
[0048]
[0049] Example 2-The high-purity m-nitrobenzaldehyde obtained in Example 6 adopts the same chromatographic detection method as that of Example 1, and the results are shown in Table 4.
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Abstract
The invention provides a synthesis method of m-nitrobenzaldehyde. The method comprises the following steps: firstly, reacting, concretely carrying out reaction on copper nitrate, water, silver nitrate and benzaldehyde in a molar ratio of (1.03-1.1):(20-40):(0.001-0.0012):1.0, so that reaction mixture is obtained; secondly, preparing an m-nitrobenzaldehyde crude product, concretely, filtering while the reaction mixture is hot, so as to obtain mother liquor, and then cooling the mother liquor, filtering, and taking solid, so that the m-nitrobenzaldehyde crude product is obtained; and thirdly, preparing high-purity m-nitrobenzaldehyde, concretely, adding a water soluble solvent into the m-nitrobenzaldehyde crude product, filtering, and drying, so that high-purity m-nitrobenzaldehyde is obtained. By adopting the method provided by the invention, molar yield of the obtained m-nitrobenzaldehyde is more than 90%, chromatographic purity is more than 99.8%, and content of o-nitrobenzaldehyde is less than 0.1%; and fewer three wastes are produced in a production process, so that the method provided by the invention is environmentally friendly.
Description
Technical field [0001] The invention relates to the technical field of organic compound synthesis, in particular to a method for synthesizing m-nitrobenzaldehyde. Background technique [0002] M-Nitrobenzaldehyde is a very important pharmaceutical intermediate, which is widely used in the synthesis of various medicines, such as closulon, cilnidipine, nitrendipine, and nimodipine. At present, there are very few domestic manufacturers. The reason is that the existing production process is complicated, the adjacent para-position selectivity is poor, and multiple recrystallizations are required to obtain qualified products. The high-purity products are not high and the amount of three wastes is large, which is very destructive to the environment. Big. [0003] Currently, the method for preparing m-nitrobenzaldehyde is as follows: [0004] Ding Chengrong et al. published an article titled "Study on the New Process of Meta-Nitrobenzaldehyde Synthesis" in 2005 in "Journal of Zhejiang Univ...
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