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A technology of nitroaniline and synthesis method, applied in the formation/introduction of nitro/nitroso group, preparation of amino compounds, chemical instruments and methods, etc., can solve problems such as environmental pollution, unsafe production process, cumbersome and complicated, and achieve The effect of simple post-processing, less environmental pollution and safe operation
Inactive Publication Date: 2015-09-30
LANZHOU UNIVERSITY
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Problems solved by technology
The existing method needs to be carried out under high temperature and high pressure conditions, and the post-treatment steps are many and cumbersome, resulting in low yield, high cost, and a large amount of difficult-to-treat wastewater; 2. The most classic method is to use concentrated nitrogen-protected aniline The mixed acid of sulfuric acid and concentrated nitric acid is used to digest and then remove the protective agent. This method is widely used in laboratories and industrial production, but this method uses strong acid, which will produce a large amount of waste acid, pollute the environment, and the production process is not safe.
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Embodiment 1
[0031] , Ts is p-toluenesulfonyl.
[0032] compound a (0.3mmol), 0.6mmol NaNO 2 and 0.2mmol potassium persulfate into the reaction vessel, add 3ml of nitromethane, and stir for 2 hours at 50°C; Volume ratio 1:10) was used as the eluent to pass through a silica gel column to obtain the product a' with a yield (98%).
Embodiment 2
[0034]
[0035] compound b (0.3mmol), 0.6mmol NaNO 2 and 0.2 mmol of potassium hydrogen persulfate were added to the reaction vessel, 3ml of nitromethane was added, and stirred at 50°C for 3 hours; (volume ratio 1:8) was used as the eluent to pass through a silica gel column to obtain products b' (50% yield) and b'' (32% yield).
Embodiment 3
[0037]
[0038] compound c (0.3mmol), 0.6mmol NaNO 2 and 0.2mmol of potassium hydrogen persulfate were added to the reaction vessel, 3ml of nitromethane was added as solvent, and stirred at 50°C for 3 hours; after the detection reaction was completed, the nitromethane was removed by rotary evaporation, and the The mixed solution (volume ratio 1:8) was used as the eluent to pass through the silica gel column to obtain the product c' with a yield of 62%.
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Abstract
The invention discloses a synthesis method of substituted nitroaniline, comprises the following steps: performing nitration on the substituted aniline and nitrite in a solvent at 20-80 DEG C to obtain the substituted nitroaniline, the structural formula of the substituted aniline is as shown in the specification, wherein R1 is p-Toluenesulfonyl, acetyl, t-butyloxycarbonyl, benzoyl, -COC(CH3)3, benzyl or methyl; R2, R3, R4, R5 and R6 are respectively and independently C1-C4 alkyl, C1-C4 alkoxy, halogen, H, NO2, OCF3 or aryloxy, at least one of R2, R4 and R6 is H, the nitration means that at least one of R2, R4 and / or R6 with value of H on the substituted aniline is substituted by NO2. The synthesis method disclosed by the invention is free from high-temperature and high-pressure, the condition is gentle, the operation is safer, the strong acid is avoided, the post-treatment is simple, and the pollution to the environment is small, and the harm is light.
Description
technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a synthesis method of substituted nitroanilines. Background technique [0002] Various substituted nitroanilines are important pharmaceutical, agricultural and chemical raw materials, and important intermediates of dyes and pigments. All along with the rapid development of the domestic organic pigment industry, more and more manufacturers have turned their attention to the production of these intermediates. In order to narrow the gap between my country's organic pigment industry and foreign countries, it is imminent to develop a more economical and advanced synthesis process for organic pigment intermediates. The preparation method of existing nitroaniline mainly contains following two kinds: 1, obtain by ammonolysis by o-chloronitrobenzene, technology is to carry out continuously in high-pressure pipeline reactor under 14.7 MPa pressure and 230 ℃ of temperature, whe...
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