Process for reducing the formation of by-product ethyl 3-(phenylamino)-2-butenoate in the production of n-acetoacetanilide
A technology of acetoacetanilide and ethyl crotonate, applied in the field of reducing the generation of by-product 3--2-ethyl crotonate, can solve problems such as easy agglomeration and poor crystal form, and achieve improved yield and, The effect of reducing consumption and preventing agglomeration
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Embodiment 1
[0030] A method for reducing by-product 3-(phenylamino)-2-butenoic acid ethyl ester in the production of N-acetoacetanilide, comprising the following steps:
[0031] Add 419.0g of 60% fresh alcohol into a 1000ml three-necked flask, cool down to 10°C, add 84.1g (1mol) of diketene and 93.1g (1mol) of aniline dropwise at the same time, naturally raise the temperature to 35°C, keep the temperature for 4 hours, then cool to 10°C ℃, filter out 388.9g alcohol mother liquor, dry to obtain N-acetoacetanilide finished product 176.7g, product yield is 99.5%, and product content is 99.8%.
[0032] The product was placed for 120 days and sieved through a 20-mesh sieve with a passing rate of 96.5%, and no caking phenomenon occurred.
Embodiment 2
[0034]Add 388.9g of the alcohol filtrate filtered out in Example 1 into a 500ml three-neck flask, add 0.93g of 31% concentrated HCl, heat up, and stop distillation when the kettle temperature reaches 98°C. 232.2 g of alcohol distillate was recovered, and the ethanol content was 68.0%. Add 119.4 g of deionized water to make 451.6 g of 50% alcohol application solution.
[0035] Add 372.5g of the above-mentioned ethanol application solution into a 1000ml three-neck flask, cool down to 10°C, add 92.5g (1.1mol) of diketene and 93.1g (1mol) of aniline dropwise at the same time, naturally raise the temperature to 50°C, keep the temperature for 4 hours, and cool to 10 DEG C, filter out 340.6g alcohol mother liquor, dry to obtain N-acetoacetanilide 176.7g, product yield is 99.5%, and product content is 99.78%.
[0036] The product was placed for 120 days, sieved with 20 meshes, the pass rate was 96.1%, and no caking phenomenon occurred.
Embodiment 3
[0038] The 340.6g alcohol filtrate filtered out in Example 2 is added in a 500ml three-necked flask, and 0.56g65% concentrated HNO is added 3 , heat up, and stop distillation when the kettle temperature reaches 98°C. 285.7 g of alcohol distillate was recovered, and the ethanol content was 57.4%. Add 78.3g of deionized water to prepare 364.0g of 45% alcohol application solution.
[0039] Add 325.9g of the above-mentioned alcohol application solution into a 1000ml three-necked flask, cool down to 10°C, and add 100.9g (1.2mol) of diketene (1.2mol) and 93.1g (1mol) of aniline dropwise at the same time, keep warm at 30°C, keep the temperature for 3 hours, and cool to 10 DEG C, filter out 291.4g alcohol mother liquor, dry to obtain N-acetoacetanilide 176.4g, product yield is 99.38%, and product content is 99.8%.
[0040] The product was placed for 120 days and sieved through a 20-mesh sieve with a passing rate of 95.9%, and no caking phenomenon occurred.
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