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Preparation process of dihydroxyanthraquinone leuco

A technology for dihydroxyanthraquinone and leuco, which is applied in the field of preparing dihydroxyanthraquinone leuco, can solve the problems of large amount of three wastes, pollution, low reduction conversion rate, etc., and achieves the effect of less three wastes, clean and environmentally friendly process

Active Publication Date: 2021-05-28
JIANGSU DAOBO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these two process routes have many deficiencies: 1. Route ① uses hydrosulfite, which is flammable and easy to decompose. It is a hazardous chemical that is difficult to control. This process is particularly strict with safety and environmental protection measures; 2. Route ① Using sodium hydrosulfite as a reducing agent in alkaline medium, a large number of by-products are generated, leuco bodies need to be washed with a large amount of soft water, the amount of three wastes is large, and the pollution is serious; 3. Route ② uses zinc powder as a reducing agent, and the reduction conversion rate is not high , a large amount of heavy metal wastewater is generated

Method used

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  • Preparation process of dihydroxyanthraquinone leuco
  • Preparation process of dihydroxyanthraquinone leuco

Examples

Experimental program
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Effect test

Embodiment 1

[0016] In a 500ml autoclave, 100g of 1,4-dihydroxyanthraquinone, 265ml of methanol, and 6g of boric acid catalyst were sequentially stirred at room temperature for 5 minutes, and then replaced with nitrogen for 5 times. Air valve, the reaction temperature is 60°C, the pressure inside the kettle is kept at 0.35MPa for 2h, adjust the hydrogen inlet valve to make the pressure inside the kettle reach 0.79MPa, keep warm for 1h, cool down to 40°C, replace with nitrogen 3 times, discharge and suction filter , washing, and drying to obtain 90 g of the target product, with a yield of 89% and a purity of 93.0%.

Embodiment 2

[0018] In a 500ml autoclave, 100g of 1,4-dihydroxyanthraquinone, 316ml of methanol, and 8g of boric acid catalyst were sequentially stirred at room temperature for 5 minutes, and then replaced with nitrogen for 5 times. Air valve, the reaction temperature is 62°C, the pressure inside the kettle is kept at 0.40MPa for 4h, adjust the hydrogen inlet valve to make the pressure inside the kettle reach 0.79MPa, keep warm for 1h, cool down to 40°C, replace with nitrogen 3 times, discharge and suction filter After the reaction, filter, wash, and dry to obtain 92.57 g of the target product. The yield is 91.8%, and the purity is 94.20%.

Embodiment 3

[0020] In a 500ml autoclave, 100g of 1,4-dihydroxyanthraquinone, 380ml of methanol, and 10g of boric acid catalyst were sequentially stirred at room temperature for 5 minutes, and then replaced with nitrogen for 5 times. Air valve, the reaction temperature is 65°C, the pressure in the kettle is kept at 0.45MPa for 5h, adjust the hydrogen inlet valve to make the pressure in the kettle reach 0.79MPa, keep warm for 1h, cool down to 40°C, replace with nitrogen 3 times, discharge and suction filter After the reaction, filter, wash and dry to obtain 93.45 g of the target product. The yield is 92.7%, and the purity is 95.60%.

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Abstract

The invention discloses a method for synthesizing a dihydroxyanthraquinone leuco body. Under a nitrogen atmosphere, 1,4-dihydroxyanthraquinone, boric acid, and methanol are sequentially put into a high-pressure reaction kettle, stirred and heated, and hydrogen gas is fed in, and the reaction is completed. Then cool down, filter with suction, wash the filter cake with water, and dry to obtain the target product 1,4-dihydroxyanthraquinone leuco. The invention adopts the solvent method, has less three wastes, the by-product is water, and the process is clean and environment-friendly.

Description

technical field [0001] The invention relates to a process for preparing dihydroxyanthraquinone leuco, belonging to the field of organic synthesis. Background technique [0002] 1,4-dihydroxyanthraquinone leuco, also known as quinizarin leuco, is an important chemical intermediate that plays an important role in the dye industry and can be widely used in solvent dyes, disperse dyes, and reactive dyes And vat dye intermediates. In recent years, this compound has been gradually applied in the research and development of pharmaceutical intermediates such as antineoplastic drugs and anticancer. Its molecular formula is C 14 h 10 o 4 , the relative molecular mass is 242.23, and the structural formula is: [0003] [0004] There are two main traditional preparation techniques for 1,4-dihydroxyanthraquinone leuco: ①Under alkaline conditions, 1,4-dihydroxyanthraquinone is used as raw material, and under the action of reducing agent hydrosulfite, reduction occurs Prepared by r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/225C07C37/07
CPCC07C37/07C07C2603/24C07C39/225
Inventor 刘学峰徐松陈路云朱止阳
Owner JIANGSU DAOBO CHEM