Continuous production process of metadiphenylacetone

Abstract

The invention belongs to the technical field of organic synthesis, and particularly relates to a continuous production process of metadiphenylacetone. The method comprises the following steps: preparing a Grignard reagent from chlorobenzene, tetrahydrofuran and magnesium chips in a nitrogen protective atmosphere in an anhydrous dry environment, transferring the Grignard reagent to a Grignard reaction kettle to react with lactate, transferring the reaction liquid generated in the reaction to a quenching kettle containing a diluted hydrochloric acid solution for quenching, and performing standing treatment after the reaction is finished; then carrying out post-treatment on the separated organic phase, adding sulfuric acid to carry out high-temperature dehydration, then cooling to 60-70 DEG C, carrying out liquid separation while hot, and recrystallizing the upper-layer product by using methanol to obtain the metadiphenylacetone. According to the preparation process, continuous and industrial production of the metadiphenylacetone is realized, less three wastes are generated, the solvent can be recycled, and the metadiphenylacetone is high in yield and purity.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a continuous production process of metaphenylacetone. Background technique [0002] The pure product of metadiphenylacetone is a colorless solid, and the industrial product is a yellow crystal. It can be used as an intermediate in the production of anticoagulant rodenticides, diquatine sodium salt, dirabatine and chlortetramone, and can also be used as a pharmaceutical intermediate for prostaglandin I2 agonists. body. [0003] Existing partial diphenylacetone synthetic route has following several kinds: [0004] 1. Starting from acetone, one-time chlorination produces monochloroacetone, and then secondary chlorination produces 1,1,1-trichloroacetone, and 1,1,1-trichloroacetone is reduced to obtain 1,1,1-trichloroacetone Chloroisopropanol, followed by phenylation to produce diphenylacetone; the reaction scheme for this method is as follows: [0005] [...

AI Technical Summary

Problems solved by technology

The recrystallization process is cumbersome and complicated, and sulfuric acid needs to be added a large amount of liquid caustic soda for neutralization reaction during the reaction process, resulting in a large amount of wastewater, which increases the pressure of wastewater treatment

[0019] In summary, the above method is only suitable for the synthesis of diphenylacetone in the laboratory, the process flow is complex, the synthesis route is long, the requirements for production equipment are high, the waste water and waste gas produced are large, and continuous production cannot be realized

Images