Preparation method for phloroglucinol

A technology of phloroglucinol and tribromobenzene is applied in the field of preparation of phloroglucinol, can solve the problems of high production cost and high total cost of final products, and achieves the effect of low production cost

Inactive Publication Date: 2012-05-16
TIANJIN SANNONGJIN TECH
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  • Summary
  • Abstract
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  • Application Information

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Problems solved by technology

The current method for preparing 1,3,5-trimethoxybenzene has high production costs, the yi

Method used

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Embodiment Construction

[0008] A preparation method of phloroglucinol, carried out according to the following steps:

[0009] 1. Mix 95% ethanol and benzene, then add 2,4,6-tribromobenzene and heat to dissolve; then gradually add concentrated sulfuric acid within 1-2 hours, stir, and keep the temperature at 50-60 degrees Celsius; then add NaNO in batches 2 Boil and keep warm for 2-3 hours; finally cool and crystallize, filter, wash with water until neutral, and dry to obtain solid 1,3,5-tribromobenzene.

[0010] 2. Mix 10g of sodium metal and 80ml of methanol to prepare sodium methoxide methanol solution, then add 80ml of dimethylformamide, then add 2g of Cu2I2 and 20g of 1,3,5-tribromobenzene, heat to 90 degrees Celsius, stir and reflux for reaction 3 Hours, filtered, and the filtrate was evaporated under reduced pressure to remove methanol and dimethylformamide. After steaming, distilled with water, the obtained distillate cooled and crystallized, filtered, and dried to obtain 1,3,5-trimethoxybenz...

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PUM

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Abstract

The invention discloses a preparation method for phloroglucinol, comprising the following steps: mixing 1, 3, 5-trimethoxy benzene and concentrated hydrochloric acid or concentrated sulfuric acid, and adding H3PO4 into them, and stirring them for 24-48 h at room temperature; adding sodium carbonate into them in batches and neutralizing them, and regulating the pH value to 2-3 and filtering them; extracting the filter liquid by ether in batches, and drying the extraction liquid and evaporating out ether to obtain yellow solid phloroglucinol. The preparation method has an advantage of low production cost. The yield of the obtained phloroglucinol is higher than 80% and purity thereof is higher than 90%.

Description

Technical field: [0001] The invention belongs to a synthesis method of a fine chemical intermediate, in particular to a preparation method of phloroglucinol. Background technique: [0002] Phloroglucinol is an important intermediate in organic synthesis, mainly used in the field of pharmaceutical manufacturing. 1,3,5-Trimethoxybenzene is a white crystalline powder, insoluble in water. The current method for preparing 1,3,5-trimethoxybenzene has high production costs, the yield is generally less than 70%, and the total cost of the final product is relatively high. Invention content: [0003] The purpose of the present invention is just to overcome the deficiencies in the above-mentioned prior art, and provide a kind of preparation method of phloroglucinol, the production cost of this method is low, the yield of obtained product is high. [0004] As mentioned above, the technical solution of the present invention is: a preparation method of phloroglucinol, which is charact...

Claims

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Application Information

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IPC IPC(8): C07C39/10C07C37/055
Inventor 韩文彬王辰王木兰张克森
Owner TIANJIN SANNONGJIN TECH
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