Preparation method of alpha-chloro-alpha-acetyl-gamma-butyrolactone

A technology of acetyl and butyrolactone, which is applied in the direction of organic chemistry, can solve the problems of toxic and harmful waste gas, great harm to the human body and the environment, and low yield of reaction, so as to reduce pollution, increase the price and increase the yield. Effect

Inactive Publication Date: 2017-04-26
LIANYUNGANG JINDUN AGROCHEMICAL CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to solve the existing α-chloro-α-acetyl-γ-butyrolactone synthesis process, a large amount of toxic and harmful sulfur dioxide, hydrochloric acid and other waste gases will be produced, which will cause great harm to the human body and the environment, and the reaction yield will be low. Problem, the present invention provides an environmentally friendly, low-cost, high-yield α-chloro-α-acetyl-γ-butyrolactone preparation method

Method used

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  • Preparation method of alpha-chloro-alpha-acetyl-gamma-butyrolactone
  • Preparation method of alpha-chloro-alpha-acetyl-gamma-butyrolactone

Examples

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Embodiment 1

[0022] In a 1000mL four-neck round bottom flask equipped with mechanical stirring, thermometer and condenser tube, add 500g of α-acetyl-γ-butyrolactone and lower it to -10°C, then pass chlorine gas at this temperature to keep the chlorine gas React in a saturated state for 5 hours, stop the chlorine gas after the reaction, and change to nitrogen gas to drive away the excess chlorine gas and hydrogen chloride gas generated by the reaction in the system, and then wash with 10% aqueous sodium bicarbonate solution to obtain 641.5g colorless α-chloro- α-acetyl-γ-butyrolactone, content 98.2%, yield 99.3%.

Embodiment 2

[0024] In a 1000mL four-neck round bottom flask equipped with mechanical stirring, thermometer and condenser tube, add 500g of α-acetyl-γ-butyrolactone and lower it to -5°C, then pass chlorine gas at this temperature to keep the chlorine gas React in a saturated state for 5 hours, stop the chlorine gas after the reaction is over, and switch to nitrogen to drive away the excess chlorine and hydrogen chloride gas generated by the reaction in the system, and then wash with 10% aqueous sodium bicarbonate to obtain 644.4g colorless α-chloro- α-acetyl-γ-butyrolactone, content 96.5%, yield 98.1%.

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Abstract

The invention discloses a preparation method of alpha-chloro-alpha-acetyl-gamma-butyrolactone. The method comprises the steps that alpha-acetyl-gamma-butyrolactone is cooled to low temperature, chlorine is introduced at the temperature, the saturation state of chlorine is kept, reacting is conducted for 5 h or above, after reacting is finished, introduction of chlorine is stopped, nitrogen is introduced to drive excess chlorine in a system and hydrogen chloride gas generated through reacting away, washing is conducted with a sodium bicarbonate aqueous solution, and a target product is obtained. Under the low temperature condition, alpha-acetyl-gamma-butyrolactone reacts with chlorine to generate the target product, a traditional chloride reagent such as sulfonyl chloride is substituted with cheap chlorine, generation of waste gas such as sulfur dioxide is avoided, the reaction time is shortened, aftertreatment of reacting is simplified, the yield of the product alpha-chloro-alpha-acetyl-gamma-butyrolactone is increased to 98% or above from 90%, the production cost is greatly lowered, and a positive effect is achieved for industrial development of prothioconazole.

Description

technical field [0001] The invention relates to a preparation method of an intermediate α-chloro-α-acetyl-γ-butyrolactone of a broad-spectrum triazolethione fungicide variety prothioconazole, belonging to the field of organic chemistry. Background technique [0002] Prothioconazole is a representative drug of triazolethione fungicides, and the mechanism of action of triazole fungicides is to inhibit the formation of fungal cell walls. Broad-spectrum, high efficiency, strong systemic property and high selectivity are the main characteristics of triazole fungicides. In addition, it can reduce the level of gibberellin in plants, eliminate the top dominance, and has the advantages of early maturity, increased production, resistance Anti-lodging, anti-lodging and other plant regulation activities. It has achieved good control effects on major diseases of grain crops such as wheat root rot, take-all, sheath blight, rice sheath blight, rice smut, and rice blast. Success has been ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/33
CPCC07D307/33
Inventor 李决武石卫兵丁斌孙毅
Owner LIANYUNGANG JINDUN AGROCHEMICAL CO LTD
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