Preparation method of dimethyl ethyl aminobenzoate midbody nitrobenzoic acid ethyl ester
A technology of ethyl dimethylaminobenzoate and ethyl nitrobenzoate, which is applied in the field of preparation of ethyl dimethylaminobenzoate intermediate p-nitrobenzoate, to reduce the amount of three wastes and reduce the cost Effect
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Embodiment 1
[0021] The reaction equation of preparing ethyl dimethylaminobenzoate intermediate p-nitrobenzoate of the present invention is as follows:
[0022] .
[0023] Concrete preparation steps are:
[0024] Add 15kg of p-nitrobenzoic acid and 60kg of ethanol into a 100L reactor, stir and dissolve, pump the metering pump into the first-stage fixed bed (temperature: 50-80°C) pre-installed with HY type solid acid catalyst, and the material coming out The content is controlled at more than 80%, and then pumped into the second-stage fixed-bed reactor (temperature 80-150°C) with a metering pump, and the content of the material coming out is more than 98%.
[0025] Put the material into the desolventizer, separate the excess ethanol and water, add 5% sodium carbonate solution to wash, wash off the excess raw material at 70-80°C, add water to disperse, centrifuge, and dry to obtain the finished product with a yield of more than 96%. .
Embodiment 2-5
[0027] The proportioning ratio of p-nitrobenzoic acid and ethanol in Examples 2-5 is shown in Table 1 below, and the other steps are the same as in Example 1, and the yields are all above 96%.
[0028]
[0029] The present invention adopts a super strong solid acid as a catalyst, and obtains the target product through the preparation method of continuous esterification in a fixed-bed reactor, which solves the problem of producing a large amount of waste acid and high-salt waste water in the existing industrial production, and greatly reduces waste water production. emission.
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