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The synthetic method of l-ethyl p-toluenesulfonyl lactylate

A technology of ethyl toluenesulfonyl lactylate and p-toluenesulfonyl chloride, which is applied in the preparation of sulfonate esters and organic chemistry, and can solve the problems of high recycling costs, difficult environmental protection and high treatment costs

Active Publication Date: 2016-01-20
JIANGSU TIANRONG GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] This process mainly uses triethylamine as an acid-binding agent, and the process is mild, so it is widely used by most manufacturers now. However, as the environmental protection requirements are getting higher and higher, triethylamine, as a foul-smelling substance, is banned and restricted in many places. , environmental protection is difficult, and the cost of treatment is high. At the same time, the recovery of triethylamine in this process is very complicated, and the recovery cost is also high, so now it is necessary to find a suitable substitute product for production

Method used

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  • The synthetic method of l-ethyl p-toluenesulfonyl lactylate
  • The synthetic method of l-ethyl p-toluenesulfonyl lactylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Put 75 grams of p-toluenesulfonyl chloride, 5 grams of anhydrous magnesium sulfate, 17 grams of sodium hydroxide and 250 ml of toluene into a 500ml four-necked reaction flask, stir and cool down to 0°C, and start to add 52 grams of L-ethyl lactate dropwise for 3 hours After the dropwise addition, keep warm at 0°C for 3 hours. After the heat preservation is over, add 100ml of water, stir for 10 minutes, let stand for stratification, remove the lower layer of water, remove the solvent by distillation under reduced pressure in the upper oil layer, and evaporate the solvent to dryness. Sent out while hot to obtain L-ethyl p-toluenesulfonyl lactylate, weighing 107 g, content 98.0%, molar yield 98.1%. Boiling point: 382~386°C (760mmHg).

Embodiment 2

[0018] Put 75 grams of p-toluenesulfonyl chloride, 5 grams of anhydrous sodium sulfate, 23 grams of potassium hydroxide and 250 ml of toluene into a 500ml four-necked reaction flask, stir and cool down to 0°C, and start to add 55 grams of L-ethyl lactate dropwise for 3 hours After the dropwise addition, keep it warm at -5°C for 3 hours. After the heat preservation is over, add 100ml of water, stir for 10 minutes, let stand to separate layers, separate the lower layer of water, remove the solvent by distillation under reduced pressure in the upper oil layer, and evaporate the solvent to dryness. , issued while hot, to obtain L-ethyl p-toluenesulfonyl lactylate, weight 108 grams, content 98.0%, molar yield 98.5%.

Embodiment 3

[0020] Put 75 grams of p-toluenesulfonyl chloride, 8 grams of anhydrous sodium sulfate, 20 grams of sodium hydroxide and 250 ml of toluene into a 500ml four-necked reaction flask, stir and cool down to 0°C, and start to add 53 grams of L-ethyl lactate dropwise for 3 hours After the dropwise addition, keep warm at 3°C ​​for 3 hours. After the heat preservation is over, add 100ml of water, stir for 10 minutes, let stand for stratification, separate the water in the lower layer, remove the solvent by distillation under reduced pressure in the upper oil layer, and evaporate the solvent to dryness. Sent out while hot to obtain L-ethyl p-toluenesulfonyl lactylate, weighing 107 g, content 98.0%, molar yield 98.1%.

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Abstract

The invention discloses a synthetic method of L-p-toluenesulfonyl ethyl lactate. The synthetic method is characterized in that para-toluensulfonyl chloride, an acid-binding agent and a catalyst are mixed in a solvent, and then cooled below 0 DEG C, then L-ethyl lactate is slowly added and then a heat-preserving reaction is carried out at a temperature ranging from -15 DEG C and 5 DEG C after addition is finished, and finally, the L-p-toluenesulfonyl ethyl lactate is obtained, wherein the acid-binding agent is sodium hydroxide or potassium hydroxide. According to the synthetic method, no repugnant substance is utilized, the L-p-toluenesulfonyl ethyl lactate having the content of more than 98% can be obtained under relatively mild conditions, and the yield of the L-p-toluenesulfonyl ethyl lactate is above 98%.

Description

technical field [0001] The invention belongs to the field of pesticide synthesis, in particular to a method for synthesizing a pesticide intermediate L-ethyl p-toluenesulfonyl lactate. Background technique [0002] L-Ethyl p-toluenesulfonyl lactate is an important intermediate of the phenoxycarboxylic acid herbicides fenoxaprop-p-p-p and quizalofop-p-p-p, and its main synthetic methods are as follows: [0003] [0004] This process mainly uses triethylamine as an acid-binding agent, and the process is mild, so it is widely used by most manufacturers now. However, as the environmental protection requirements are getting higher and higher, triethylamine, as a foul-smelling substance, is banned and restricted in many places. , environmental protection is difficult, and the cost of treatment is high. At the same time, the recovery of triethylamine in this process is very complicated, and the recovery cost is also high. Therefore, it is now necessary to find a suitable substit...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/73C07C303/28
Inventor 许网保臧伟新魏明阳虞国新
Owner JIANGSU TIANRONG GROUP