Environment-friendly preparation process of N-(4-ethoxy carbonyl phenyl)-N'-methyl-N'-phenyl formamidine intermediate
A technology of ethoxycarbonylphenyl and phenylformamidine, which is applied in the field of fine chemicals, can solve problems such as environmental pollution, lower esterification yield, large and high-salt wastewater, etc., to reduce production costs, reduce pollution, and improve esterification. The effect of chemical reaction yield
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example 1)
[0025] This example is the ethanol recovery treatment method that collects in step 3. and step 4. of comparative example 1:
[0026] First, carry out rectification on the collected ethanol to obtain preliminary recovered ethanol with a purity of 96% to 97%; then add sodium hydroxide (the addition amount is about 1% of the weight of ethanol) to the preliminary recovered ethanol, heat to reflux, Insulate for 2 hours; finally start atmospheric distillation, collect fractions, stop heating when the internal temperature reaches 85°C, and obtain recycled ethanol with a purity ≥ 99.5%.
Embodiment 1)
[0028] This embodiment is a green preparation process of N-(4-ethoxycarbonylphenyl)-N'-methyl-N'-phenylformamidine intermediate, and the specific steps are as follows:
[0029] ①Put 80kg of commercially available anhydrous ethanol (1.74kmol) into the reaction kettle, then add 50kg of p-nitrobenzoic acid (0.30kmol) and 10kg of commercially available concentrated sulfuric acid (0.10kmol) while stirring, and stir after adding Heat up to 80±2°C, reflux for 6h.
[0030] After the reaction is finished, ethanol is distilled out at normal pressure first, and when it is steamed to 95-98°C, the ethanol is distilled out under reduced pressure.
[0031] Move the upper catalyst layer (that is, the concentrated sulfuric acid layer) to the still, and distill under reduced pressure (vacuum degree <-0.09MPa). After steaming to 120-122°C, control the temperature to distill until anhydrous distills out to obtain Recycling concentrated sulfuric acid.
[0032] Keep the lower organic layer warm a...
Embodiment 2)
[0036] The rest of this embodiment are the same as in Example 1, except that the concentrated sulfuric acid used in step 1. is the recovered and processed concentrated sulfuric acid obtained according to the recovery and treatment method in step 1. Sulfuric acid), the reaction results are shown in Table 1.
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