Green synthesis process for p-chloro-o-nitroacetoanilide
A technology of chloroacetoacetanilide and green process is applied in the field of green process for synthesizing o-nitro-p-chloroacetoacetanilide, and can solve the problems that mother liquor cannot be applied mechanically, product purity is not high, etc., and achieves shortened reaction time, no solid waste generation, The effect of solubility enhancement
Inactive Publication Date: 2013-11-27
JIANGSU LONGCHANG CHEM
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Problems solved by technology
The disadvantage of this method is that the product purity is not high, and the mother liquor cannot be applied mechanically
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[0018] In order to make the object, technical solution and beneficial effect of the present invention clearer, the present invention adopts the following specific examples to describe the technical solution of the present invention in detail.
[0019] Add a mixed solvent into the reaction kettle, add 1000kg of toluene, 0.4kg of pyridine, start stirring, add 400kg of p-chloro-o-nitroaniline, raise the temperature to 60°C, start to add 250kg of diketene dropwise, and complete the dropwise addition within 60°C. Continue to keep warm for 2 hours after completion. After the reaction is completed, cool down to 0°C, filter, and dry the filter cake. The yield reaches 99%.
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The invention discloses a green synthesis process for p-chloro-o-nitroacetoanilide. The process comprises the following steps of mixing a novel mixed catalyst system and p-chloro-o-nitroaniline, and enabling the novel mixed catalyst system and the p-chloro-o-nitroaniline to dissolve, wherein the mole ratio of the p-chloro-o-nitroaniline to diketene is 1: (1.05-1.5); finishing the dropwise adding operation of the diketene within 3h; and continuing to react at the temperature of 90 DEG C for 4h to obtain the p-chloro-o-nitroacetoanilide. The solubility of the p-chloro-o-nitroaniline in a solvent is improved, the yield of products is high, the reaction time is shortened, the solvent dosage is reduced, and no solid wastes are generated.
Description
technical field [0001] The invention relates to a green process for synthesizing o-nitro-p-chloroacetoacetanilide, which belongs to the technical field of compound preparation. Background technique [0002] O-nitro-p-chloroacetoacetanilide is a light yellow crystal, which is mainly used as an intermediate in the synthesis of herbicides and drugs. [0003] US4636562 discloses taking p-chloro-o-nitroaniline as a raw material, triethylamine as a catalyst, backflowing and dripping a mixed solution of diketene and benzene in benzene, after the reaction finishes, the crude product is recrystallized with ethanol, and the process yield is not high, and Recrystallization produces a large amount of effluent. [0004] EP0280156 discloses a kind of using p-chloro-o-nitroaniline as a raw material, and using potassium fluoride as a catalyst under acetic acid as a solvent to react at a certain temperature. The shortcoming of this method is that product purity is not high, and mother liq...
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IPC IPC(8): C07C235/80C07C231/04
Inventor 赵雪松吴春江王兆昌佘卫民
Owner JIANGSU LONGCHANG CHEM
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