Continuous production process of metadiphenylacetone

A technology for producing diphenylacetone and its production process, which is applied in the field of continuous production process of diphenylacetone, can solve the problems of complex process flow, excessive waste water and waste gas, and high requirements for production equipment, and achieve high yield and purity, Effect of shortening operation time and reducing production cost

Active Publication Date: 2020-11-03
ZHANGJIAGANG JIULI NEW MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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

Method used

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  • Continuous production process of metadiphenylacetone
  • Continuous production process of metadiphenylacetone

Examples

Experimental program
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Effect test

Embodiment 1

[0047] The continuous production process of the partial diphenylacetone described in the present embodiment 1 is made up of the following steps:

[0048] (1) Under a nitrogen protective atmosphere and an anhydrous dry environment, place 1.7Kg of prefabricated Grignard reagent as an initiator in a Grignard reagent kettle, then add 15.8Kg of anhydrous tetrahydrofuran and 3.5Kg of magnesium chips, heat to slight reflux, drop Add anhydrous tetrahydrofuran solution of chlorobenzene (chlorobenzene 15.2Kg, THF 22.5Kg), keep the reaction system under slight reflux, and prepare the Grignard reagent; after the dropwise addition, continue to react for 4.5 hours, then lower the temperature to room temperature and let stand; The prepared Grignard reagent is transported to the Grignard reactor through pipelines;

[0049] (2) Add 6.4Kg of lactic acid ester to the Grignard reaction kettle, reflux at 105°C for 2 hours, cool down to 10°C, transfer the reaction solution generated by the reaction...

Embodiment 2

[0061] The continuous production process of the partial diphenylacetone described in the present embodiment 2 is made up of the following steps:

[0062] (1) Under a nitrogen protective atmosphere and an anhydrous dry environment, place 1.9Kg of prefabricated Grignard reagent as an initiator in a Grignard reagent kettle, then add 17.2Kg of anhydrous tetrahydrofuran and 3.8Kg of magnesium chips, heat to slight reflux, drop Add anhydrous tetrahydrofuran solution of chlorobenzene (chlorobenzene 17.0Kg, THF 24.4Kg), keep the reaction system under slight reflux, and prepare the Grignard reagent; after the dropwise addition, continue to react for 6 hours, then lower the temperature to room temperature and let stand; The prepared Grignard reagent is transported to the Grignard reactor through pipelines;

[0063] (2) Add 7.0Kg of lactic acid ester to the Grignard reaction kettle, reflux at 100°C for 2.5 hours, cool down to 5°C, transfer the reaction solution generated by the reaction ...

Embodiment 3

[0075] The continuous production process of the partial diphenylacetone described in the present embodiment 3 is made up of the following steps:

[0076] (1) Under a nitrogen protective atmosphere and an anhydrous dry environment, place 1.5Kg of prefabricated Grignard reagent as an initiator in a Grignard reagent kettle, then add 13.5Kg of anhydrous tetrahydrofuran and 3.0Kg of magnesium chips, heat to slight reflux, drop Add anhydrous tetrahydrofuran solution of chlorobenzene (chlorobenzene 13.5Kg, THF 19.2Kg), keep the reaction system under slight reflux, and prepare the Grignard reagent; after the dropwise addition, continue to react for 3 hours, then lower the temperature to room temperature and let stand; The prepared Grignard reagent is transported to the Grignard reactor through pipelines;

[0077] (2) Add 5.5Kg of lactic acid ester to the Grignard reaction kettle, reflux at 95°C for 3.0 hours, cool down to 0°C, transfer the reaction solution generated by the reaction t...

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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] [...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/52C07C49/215
CPCC07C29/36C07C45/52C07C49/215C07C33/26
Inventor 苏旭吴茂江闫晗邓金标石卫民
Owner ZHANGJIAGANG JIULI NEW MATERIAL TECH CO LTD
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