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Continuous Production Process of Diphenylacetone

A technology for the production of diphenylacetone and its production process, which is applied in the field of continuous production process of diphenylacetone, can solve the problems of high requirements for production equipment, complex process flow, waste water and waste gas, etc., so as to reduce production costs and shorten Operation time, yield and high purity effect

Active Publication Date: 2021-04-23
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 Diphenylacetone
  • Continuous Production Process of Diphenylacetone

Examples

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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 in particular relates to a continuous production process of metaphenylacetone. Firstly, under a nitrogen protective atmosphere and an anhydrous dry environment, the Grignard reagent was prepared by using chlorobenzene, tetrahydrofuran and magnesium chips, and then the Grignard reagent was transferred to the Grignard reactor to react with lactate, and the reaction solution generated by the reaction was transferred to Quenching is carried out in a quenching kettle filled with dilute hydrochloric acid solution. After the reaction is completed, stand still for liquid separation. The separated organic phase is post-treated, and sulfuric acid is added for high-temperature dehydration. The upper layer product was recrystallized from methanol to obtain partial diphenylacetone. The preparation process realizes the continuous and industrialized production of the partial diphenylacetone, produces less three wastes, the solvent can be reused after being recovered, and the yield and purity of the prepared partial diphenylacetone are high.

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 Patents(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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