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A kind of synthetic method of 1,4-dihydroxyanthraquinone leuco

A technology of dihydroxyanthraquinone and synthesis method, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of unguaranteed process safety, rising procurement and storage costs, insufficient stability of hydrosulfites, etc. To achieve the effect of shortening the reaction maintenance time, good economic and environmental benefits, qualified and stable quality

Active Publication Date: 2021-10-29
安徽清科瑞洁新材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The characteristic of this process is that the raw materials are easy to obtain, but the main disadvantage is that sodium carbonate or sodium bicarbonate is often used as the alkaline medium for the reaction, and the hydrosulfite is not stable enough. Because a large amount of foam is easily generated in the decomposition system, the safety of the process cannot be guaranteed, and the storage environment is harsh. Poor site environment, resulting in increased procurement and storage costs
In addition, the reaction conversion rate of hydrosulfite is low, the reaction maintenance time is long, the production efficiency is low, and the cost is also virtually increased.

Method used

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  • A kind of synthetic method of 1,4-dihydroxyanthraquinone leuco

Examples

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Effect test

Embodiment 1

[0020] This example provides a kind of synthetic method of 1,4-dihydroxyanthraquinone leucosome, and it comprises the following steps:

[0021] (a) Add 60ml of water, 20g of 30% liquid caustic soda, and 20g of 1,4-dihydroxyanthraquinone in sequence in a four-neck flask, heat up and stir, and keep the temperature at 70°C~75°C for 30min to make 1,4-dihydroxyanthraquinone Quinone and fully dissolved;

[0022] (b) Slowly add 6g of thiourea under stirring. After SL is added, raise the temperature to 88°C for 2 hours, cool down, and detect the reaction end point by HPLC; after the end point is reached, filter, wash with hot water until neutral, and dry the filter cake to obtain the finished product 19.2 g, content 95.64%, yield 96.0%.

Embodiment 2

[0024] This example provides a synthesis method of 1,4-dihydroxyanthraquinone leucosome, which is basically the same as that in Example 1, the difference is that the amount of water added in step (a) is 120ml, and finally filtered and washed with hot water To neutrality, the filter cake was dried to obtain 18.6g of finished product, the content was 95.22%, and the yield was 93.0%.

Embodiment 3

[0026] This example provides a kind of synthetic method of 1,4-dihydroxyanthraquinone leucosome, which is basically the same as that in Example 1. The difference is that the input amount of liquid caustic soda in step (a) is 30g, and finally after filtering, heat Wash with water until neutral, and dry the filter cake to obtain 17.8 g of the finished product, with a content of 96.13% and a yield of 89.0%.

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Abstract

The patent of the present invention relates to a synthesis method of 1,4-dihydroxyanthraquinone leuco body. By using liquid caustic soda as an alkaline medium, it solves the phenomenon of a large number of bubbles and even floating materials in the reaction process, which greatly improves the The operating environment is improved; the use of SL as a reducing agent solves the problems of difficult storage of sodium hydrosulfite, potential safety hazards in the reaction, and low conversion rate, improving the conversion rate and reducing potential safety hazards; improving the feeding sequence, making the reaction more complete and shortening the reaction time The maintenance time greatly improves the production efficiency.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis and relates to a new reduction synthesis process, in particular to a synthesis method of 1,4-dihydroxyanthraquinone leuco. Background technique [0002] 1,4-dihydroxyanthraquinone leuco is a kind of important chemical intermediate, before the present invention, the existing technique of chemically synthesizing 1,4-dihydroxyanthraquinone leuco is in alkaline medium, uses Sodium hydrosulfite reduces 1,4-dihydroxyanthraquinone to produce 1,4-dihydroxyanthraquinone leuco. [0003] The characteristic of this process is that the raw materials are easy to obtain, but the main disadvantage is that sodium carbonate or sodium bicarbonate is often used as the alkaline medium for the reaction, and sodium hydrosulfite is not stable enough. Because a large amount of foam is easily generated in the decomposition system, the safety of the process cannot be guaranteed, and the storage environment is hars...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C37/07C07C39/12
CPCC07C37/07C07C39/12
Inventor 周利霞刘镛李成
Owner 安徽清科瑞洁新材料有限公司
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