Green synthesis process for p-chloro-o-nitroacetoanilide

Abstract

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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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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