A kind of preparation method of prohexadione calcium

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

Active Publication Date: 2020-10-13
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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  • A kind of preparation method of prohexadione calcium
  • A kind of preparation method of prohexadione calcium

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preparation example Construction

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

[0024] Prepare a calcium acetate aqueous solution with a concentration of 20-30% by mass, and add 3,5-dioxo-4-propionylcyclohexanecarboxylic acid ethyl ester to the calcium acetate aqueous solution, where the aqueous solution and 3,5-dioxo The mass ratio of ethyl -4-propionylcyclohexanecarboxylate is 10-20:1, add 0.5-2% of the total mass of lipase catalyst, and react at 30-80℃ and 250-800 revolutions per minute. After 2-10 hours, the lipase catalyst was recovered by filtration, and white solid calcium 3,5-dioxo-4-propionylcyclohexane carboxylate was precipitated out by cooling.

Embodiment 1

[0026] Add 20 grams of calcium acetate to 80 grams of water to make a 20% solution. Add the calcium acetate aqueous solution to a 250ml three-neck flask with stirring, and add 10 grams of 3,5-dioxo-4-propionylcyclohexane carboxylate Ethyl acid, 0.55g Novozyme435, reacted at 30℃, 250-rpm stirring speed for 10 hours, filtered and recovered the lipase catalyst Novozyme435, and cooled to precipitate white 3,5-dioxo-4-propionylcyclohexane Calcium carboxylate, dried, weighed 9.5 grams, 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 make a 30% solution. Add the calcium acetate aqueous solution to a 250ml three-neck flask with stirring, and add 20 grams of 3,5-dioxo-4-propionylcyclohexane carboxylate Lipozyme RMIM, 2.4 g lipozyme RMIM, react for 2 hours at 80°C and 800 rpm stirring speed, filter and recover the lipase catalyst lipozyme RMIM, cooling to precipitate white 3,5-dioxo-4-propionyl cyclohexane The calcium carboxylate was dried and weighed to obtain 18.8 g, with a yield of 97.6% and an HPLC content of 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 calcium regalicum, belonging 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 as natural plant hormones and natural plant hormones extracted from organisms. Calcium hexadione 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 calcium cyclamate is mainly used to control the growth of cereal crops, 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. [0006] In recent year...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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