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One-pot synthesis technology of photo initiator 2,4-diethylthioxanthone

A technology of diethylsulfide and xanthone, which is applied in the technical field of one-pot synthesis of photoinitiator 2,4-diethylthioxanthone, which can solve the problem of low equipment utilization and labor efficiency, and the appearance of products containing Problems such as variegated color and difficult post-processing can be achieved to improve product quality, reduce raw material costs, and increase single-pot efficiency.

Inactive Publication Date: 2020-02-28
JIAN DONGQING FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This process not only has high reaction temperature and many side reactions (especially some sulfonated aromatic compounds), the appearance of the product contains variegated colors, the appearance is poor, such as a small amount of red impurities on the appearance of the product, and the post-treatment is very difficult, requiring multiple treatments , product distillation and other steps, the work intensity is high, the utilization rate of equipment and labor efficiency are very low

Method used

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  • One-pot synthesis technology of photo initiator 2,4-diethylthioxanthone

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Add 40 ml of concentrated sulfuric acid, 100 g of dithiosalicylic acid, and 8 g of polyphosphoric acid into a 500 ml four-necked reaction flask, cool to below 0°C in an ice-salt bath while stirring, and add 1,3-diethylbenzene dropwise 100 grams, the reaction temperature is controlled not to exceed 5°C. After the addition, the ice-salt bath was removed, and the temperature was naturally raised to room temperature, and the reaction was continued for 1 hour. Replace the oil bath, slowly raise the temperature to 65° C., and react at 65° C. for 5 hours. Follow the reaction by HPLC until the reaction of dithiosalicylic acid is complete. Cool the reaction product, add 90 grams of 1,3-diethylbenzene and 60 grams of water, stir for half an hour, let stand to separate the phases, wash the organic phase with alkali and water, concentrate, and then cool to 5°C overnight, the next day Filtrate, wash the filter cake with a small amount of ice ethanol, and vacuum-dry to obtain 150 gr...

Embodiment 2

[0030] Add 40 ml of concentrated sulfuric acid, 2 g of phosphorus pentoxide and 16 g of methanesulfonic acid into a 500 ml four-necked reaction flask, stir evenly, then add 100 g of thiosalicylic acid, and cool to 0°C in an ice-salt bath while stirring Next, 100 grams of 1,3-diethylbenzene was added dropwise, and the reaction temperature was controlled not to exceed 5°C. After the addition, the ice-salt bath was removed, and the temperature was naturally raised to room temperature, and the reaction was continued for 1 hour. Put on an oil bath, slowly heat up to 65°C, react at 65°C for 5 hours, follow the reaction by HPLC until the reaction of dithiosalicylic acid is complete, cool down, add 90 grams of toluene, 60 grams of water, stir for half an hour, and wait The phases were separated, and the organic phase was washed with alkali and water, and concentrated. Add anhydrous methanol and activated carbon to the residue, raise the temperature to 45°C and stir for half an hour, ...

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Abstract

The invention discloses a one-pot synthesis technology of a photo initiator 2,4-diethylthioxanthone. The invention belongs to the field of fine chemical engineering, and specifically relates to a one-pot synthesis technology of a photo initiator 2,4-diethylthioxanthone. According to the technology, thiosalicylic acid (or dithiosalicylic acid) and 1,3-diethylbenzene are taken as the raw materials,concentrated sulfuric acid is taken as a catalyst and a solvent, and under the action of a co-catalyst, condensation reactions are carried out for 4 to 8 hours at a temperature of 0-70 DEG C. Post treatment technologies (condensation, extraction, concentration, and recrystallization) are carried out in one reaction unit; the obtained product is filtered and dried to obtain high purity 2,4-diethylthioxanthone. The technology has the advantages of good selectivity, low reaction temperature, short reaction time, high yield, simple and convenient operation, and high efficiency of single kettle, the equipment investment, the energy consumption, the operation strength, and the production cost are reduced, and the technology is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of fine chemical industry, and exactly relates to a process for synthesizing photoinitiator 2,4-diethylthioxanthone in one pot, using thiosalicylic acid or dithiosalicylic acid, 1,3 -Diethylbenzene is used as the raw material, concentrated sulfuric acid is used as the catalyst and solvent, and under the action of the co-catalyst, the condensation, extraction, concentration, recrystallization and other processes are concentrated in the same reaction device to complete, and the obtained product is filtered and dried , and finally high-purity 2,4-diethylthioxanthone was obtained. The invention has the advantages of good selectivity, low reaction temperature, short reaction time, high yield, simple operation, high single-pot efficiency, etc., reduces equipment investment, operation intensity and production cost. Background technique [0002] Thioxanthone (also called thioxanthone) compounds are often used as photoinitiat...

Claims

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Application Information

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IPC IPC(8): C07D335/16
CPCC07D335/16
Inventor 曽孝军
Owner JIAN DONGQING FINE CHEM
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