Preparation method of 4-amino-benzoyl formic-N-(4-amino-benzoyl formic) amine

Abstract

The invention relates to a preparation method of 4-amino-benzoyl formic-N-(4-amino-benzoyl formic) amine, which belongs to the technical field of the compound preparation method. The invention particularly relates to a preparation method of an organic pigment intermediate, which is characterized by comprising the following steps that: Para Amino Benzamide and paranitrobenzoyl chloride have condensation reaction in solvent under the condition that alkali carbonate exists to obtain 4-nitrobenzoyl-N-(4-nitrobenzoyl)amine; the 4-nitrobenzoyl-N-(4-nitrobenzoyl)amine is catalyzed and reduced by hydrazine hydrate in the solvent to obtain 4-amino-benzoyl formic-N-(4-amino-benzoyl formic) amine. So far, the preparation method not only improves the purity of the product to more than 99.7 percent, but also improves the total yield to more than 93.2 percent, and improves the quality and the yield of the product. During the synthesis process, the productivity of three wastes is reduced to less than 2 tons of waste water every one ton of product, so the process has industrialized value.

Description

technical field [0001] The invention belongs to the technical field of compound preparation methods, and in particular relates to a preparation method of an organic pigment intermediate. Background technique [0002] Organic Pigment Yellow C.I 181# is a high-grade organic pigment with good performance, and 4-aminobenzoyl-N-(4-aminobenzoyl)amine is an important raw material for the synthesis of Organic Pigment Yellow C.I 181#. So far, 4-aminobenzoyl-N-(4-aminobenzamide) amine, as an intermediate, has only been industrialized in a few countries such as Germany and the United States in the world, and the process steps are relatively complicated and costly. high. With the continuous deepening of international research on the application of organic pigment yellow C.I 181# in recent years, the pigment has also been paid more and more attention by the business community, and has shown an unprecedented active state in the research field in the past two years. [0003] However, the...

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Problems solved by technology

[0003] However, there are still few reports on the synthesis of 4-aminobenzoyl-N-(4-aminobenzamide) amide in the existing relevant literature, and two relevant documents of DE 2.845.947 and CN 1869003 are included in the American Chemical Abstracts, And there is only one related report (Synth.Commun; EN32,82002) in Beil., although the synthetic method adopted in it has reached the degree that can be industrialized in yield and product quality, but the catalyst loading hydrogenation that he adopts makes process Complicated and costly