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Synthesis method of 2,8-dimethyl phenoxathiin

A technology of dimethylphenoxadiene and dimethylphenoxane, which is applied in the fields of medicine and chemical industry, can solve the problems of affecting usage and dosage promotion, large discharge of three wastes, and high production costs, and achieve obvious economic and environmental benefits, reducing Emission amount, effect of side reaction control

Inactive Publication Date: 2015-05-27
扬州市天平化工厂有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the prior art, the synthesis process of 2,8-methylphenoxathione has high production cost, low purity, large discharge of three wastes, high technical difficulty and harsh conditions, which greatly affect its use and dosage promotion

Method used

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  • Synthesis method of 2,8-dimethyl phenoxathiin

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preparation example Construction

[0019] The invention discloses a synthesis method of 2,8-dimethylphenoxathione, and the synthesis method comprises the following preparation steps:

[0020] (1) Condensation reaction: Add 4,4-dimethyldiphenyl ether into the reaction pot, put in anhydrous aluminum trichloride at 40°C, add sulfur powder in batches under stirring, and control the temperature at 55-60°C After 1-1.5 hours of heat preservation, the temperature was raised to 105-110°C, the heat preservation reaction was carried out for 2-3 hours, and the temperature was lowered to below 40°C to obtain a reaction liquid, and then anhydrous dichloromethane and glacial acid water were added to the reaction liquid, and the temperature was controlled at Below 40°C, stir for 1 hour after addition, stand for stratification, neutralize the organic layer with alkaline solution to PH=6-7, continue to stand for stratification, then wash the organic layer with water, separate the organic layer and transfer to precipitation Pot, ...

Embodiment 1

[0024] Condensation reaction: Add 450kg of 4,4-dimethyldiphenyl ether into the reaction pot, put 200kg of anhydrous aluminum trichloride at 40°C, add 50kg of sulfur powder in batches under stirring, and control the temperature at 55-60°C After 1-1.5 hours of heat preservation, the temperature is raised to 105-110°C, the heat preservation reaction is carried out for 2-3h, and the temperature is lowered to below 40°C to obtain a reaction solution, and then 1000kg of anhydrous dichloromethane and 1000kg of glacial acid water (wherein , hydrochloric acid 250kg, water 750kg), control the temperature below 40 ° C, add and stir for 1 hour, stand and separate, the organic layer is neutralized to PH=6-7 with 200L of 20% sodium carbonate solution, continue to stand and separate, Then wash the organic layer with 1000L of water, separate the organic layer and transfer it to a desolventizer to remove dichloroethane to obtain a crude reaction product, which is fractionated in vacuum, and the...

Embodiment 2

[0027] Condensation reaction: Add 950kg of 4,4-dimethyldiphenyl ether into the reaction pot, put 450kg of anhydrous aluminum trichloride at 40°C, add 100kg of sulfur powder in batches under stirring, and control the temperature at 55-60°C After 1-1.5 hours of heat preservation, the temperature is raised to 105-110°C, the heat preservation reaction is carried out for 2-3h, and the temperature is lowered to below 40°C to obtain a reaction solution, and then 2000kg of anhydrous dichloromethane and 2000kg of glacial acid water (wherein , hydrochloric acid 500kg, water 1500kg), control the temperature below 40°C, add and stir for 1 hour, stand for stratification, use 400L 20% potassium carbonate H=6-7 for organic, continue to stand for stratification, and then use 2000L of clear water Wash the organic layer, separate the organic layer and transfer it to a desolventizing pot to remove dichloroethane to obtain a crude reaction product, which is subjected to vacuum fractionation, and t...

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Abstract

The invention discloses a synthesis method of 2,8-dimethyl phenoxathiin. The synthesis method comprises the following steps of adding 4,4-dimethyl diphenyl ether into a reaction pot, adding anhydrous aluminum trichloride into the reaction pot at a temperature within 40 DEG C, adding sulfur powder into the reaction pot in batches with stirring, carrying out a condensation reaction process, carrying out aftertreatment, and carrying out vacuum fractionation of a crude product to obtain a crude product of 2,8-dimethyl phenoxathiin, adding the crude product of 2,8-dimethyl phenoxathiin into methanol for recrystallization, cooling to a temperature of 0 DEG C, carrying out heat preservation for 5-6h, and carrying out centrifugation, decompression, and drying to obtain a finished product of 2,8-dimethyl phenoxathiin. The synthesis method reduces a condensation reaction temperature, shortens reaction time, controls the incidence of a side reaction, improves a product yield, reduces a production cost, reduces a discharge amount of three wastes in the whole process, and satisfies production requirements of environmental protection and cleanness.

Description

technical field [0001] The invention relates to the technical fields of medicine and chemical industry, in particular to a method for synthesizing 2,8-dimethylphenoxathione. Background technique [0002] 2. 8-Dimethylphenoxathione, whose structural formula is shown in the following formula (I), has a light yellow powder solid appearance, and is an important pharmaceutical intermediate of a class of episulfide-like derivatives, which can exist in different pharmacological effects In the molecular structure of pharmaceuticals, it is mainly used to synthesize drugs that soften blood vessels and promote metabolism. In the prior art, the synthesis process of 2,8-methylphenoxathione has high production cost, low purity, large discharge of three wastes, high technical difficulty and harsh conditions, which greatly affect its use and dosage promotion. [0003] Contents of the invention [0004] The technical problem mainly solved by the present invention is to provide a synthe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D327/08
Inventor 吕欢欢马文元张兴华
Owner 扬州市天平化工厂有限公司