Preparation method of prohexadione calcium

A technology of prohexadione calcium and calcium acetate, applied in chemical recovery, fermentation and other directions, can solve the problems of low total yield and cumbersome process, and achieve the effect of high yield

Active Publication Date: 2019-04-26
浙江大鹏药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process is cumbersome and produces a large amount of waste liquid. Although a white solid with high purity is obtained, the total yield is low

Method used

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  • Preparation method of prohexadione calcium

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preparation example Construction

[0023] A preparation method of prohexadione calcium is as follows:

[0024] Prepare a calcium acetate aqueous solution with a concentration of 20-30% by mass, add 3,5-dioxo-4-propionylcyclohexanecarboxylate ethyl ester to the calcium acetate aqueous solution, wherein the aqueous solution is mixed with 3,5-dioxo - The mass ratio of ethyl 4-propionylcyclohexanecarboxylate is 10-20:1, add 0.5-2% lipase catalyst in total mass, and react at 30-80°C and 250-800 r / min stirring speed After 2-10 hours, the lipase catalyst was recovered by filtration, and the white solid calcium 3,5-dioxo-4-propionylcyclohexanecarboxylate was precipitated by cooling down.

Embodiment 1

[0026] Add 20 grams of calcium acetate to 80 grams of water to form a 20% solution, add the calcium acetate aqueous solution to a 250ml three-necked flask with stirring, add 10 grams of 3,5-dioxo-4-propionylcyclohexanecarboxylate Ethyl acid, 0.55 g Novozyme 435, react at 30°C, 250-r / min stirring speed for 10 hours, filter and recover the lipase catalyst Novozyme 435, cool down to precipitate white 3,5-dioxo-4-propionylcyclohexane Calcium carboxylate, dried, weighed to obtain 9.5 g, yield 98.7%, HPLC content 98.7%, IR (cm -1 ): 2889.1, 1645.2, 1561.1, 1381.3.

Embodiment 2

[0028] Add 30 grams of calcium acetate to 70 grams of water to form a 30% solution, add the calcium acetate aqueous solution to a 250 ml three-necked flask with stirring, add 20 grams of 3,5-dioxo-4-propionylcyclohexanecarboxylate Acetate ethyl ester, 2.4 g lipozyme RMIM, react at 80 ° C, 800 r / min stirring speed for 2 hours, filter and recover the lipase catalyst lipozyme RMIM, cool down and separate out white 3,5-dioxo-4-propionylcyclohexane Calcium carboxylate was dried and weighed to obtain 18.8 g, the yield was 97.6%, and the HPLC content was 98.5%.

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Abstract

The invention discloses a preparation method of prohexadione calcium. The preparation method comprises the following steps: preparing a calcium acetate aqueous solution with mass percentage concentration of 20-30%, adding 3,5-dioxo-4-propionyl ethyl cyclohexane carboxylate into the calcium acetate aqueous solution, wherein a mass ratio of the aqueous solution to the 3,5-dioxo-4-propionyl ethyl cyclohexane carboxylate is (10 to 20) : 1; adding a lipase catalyst which accounts for 0.5-2% of the total mass, reacting for 2-10 hours at a temperature of 30-80 DEG C under stirring speed of 250-800 revolutions per minute, filtering and recycling the lipase catalyst, and cooling to separate out 3,5-dioxo-4-propionyl ethyl cyclohexane carboxylate, wherein the lipase catalyst is Novozyme 435, lipozyme RMIM or Lipozyme TLIM. The method does not use an organic solvent, is environmentally friendly, is high in yield and is high in purity.

Description

technical field [0001] The invention relates to a preparation method of prohexadione calcium, which belongs to the technical field of pesticide synthesis. Background technique [0002] Plant growth regulators are a class of pesticides used to regulate plant growth and development, including synthetic compounds with similar effects to natural plant hormones and natural plant hormones extracted from organisms. Prohexadione calcium is a new type of cyclohexenone plant growth regulator, its common name is: prohexadione-Calcium. The chemical name is: calcium 3,5-dioxo-4-propionylcyclohexene carboxylate. The English name is: Calcium 3,5-dioxo-4-propionylcyclohexanecarboxylic acid. [0003] The structural formula is: [0004] [0005] The role of prohexadione is mainly used to control the growth of cereal crops, which can shorten the length of crop stems, and can enhance the plant's disease resistance, cold resistance, and stress resistance, and has obvious lodging resistance...

Claims

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Application Information

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IPC IPC(8): C12P7/40
CPCC12P7/40Y02P20/584
Inventor 蒋成君徐大国徐学春王自田
Owner 浙江大鹏药业股份有限公司
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