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Method for preparing thidiazuron

A technology of thiadizuron and thiadiazole, which is applied in the field of preparation of plant growth regulators, can solve the problems of high solvent price, unreported product purity, and high production cost, and achieve the effects of low price, easy industrial production, and easy solvent

Active Publication Date: 2009-03-18
江苏省农用激素工程技术研究中心有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Chinese patent CN1196354 improves the method of the U.S. patent. It controls the reaction temperature at 8-12°C, and the reaction is allowed to stand for 24 hours. The yield can reach 88.74%, and the product purity is not reported.
Although this method has solved the purity problem of thiadizuron, the production cost is higher because the price of the solvent used is too high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The preparation method of the Thidiazuron of the present embodiment is as follows:

[0015] ①Add 50.5g of reactant 5-amino-1,2,3-thiadiazole (0.5mol) into 200ml of solvent methyl ethyl ketone under stirring, and continue stirring for about 10min until 5-amino-1,2,3 - Thiadiazole is completely dissolved.

[0016] ②Add 64g of reactant phenyl isocyanate (0.53mol) and 0.5ml of catalyst triethylamine (0.003mol) to the solution, and make 5-amino-1,2,3 -Thiadiazole and phenyl isocyanate undergo a catalytic synthesis reaction, the reaction time is 3h, then cooled to 20°C, and then stirred for 1h to make it completely reacted, filtered to obtain 102g of the target product thiadizuron, and the mother liquor was recovered (after drying, apply mechanically ), the yield reaches 92.7%, and the product purity reaches 98.5%.

Embodiment 2～ Embodiment 6

[0018] Each embodiment is basically the same as Embodiment 1, and the differences are shown in Table 1.

[0019] Table 1

[0020] Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 5-amino-1,2,

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PUM

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Abstract

The invention disclosed a method for preparing Thidiazuron. The method comprises the following steps: (1) adding a reactant of 5-amino-1, 2, 3-thiadiazole to a butanone solvent while stirring, keeping stirring the mixed solution until the 5-amino-1, 2, 3-thiadiazole is completely dissolved; (2) adding reactants of phenyl isocyanate and a triethylamine catalyst to the solution obtained in the step (1), so that the 5-amino-1, 2, 3-thiadiazole has catalytic synthesis reaction with the phenyl isocyanate, and then filtering the reactant after the reaction is complete to obtain a filter cake which is the Thidiazuron finished product. With the method, the yield of the Thidiazuron can be more than 92 percent and the purity can be more than 98 percent; besides, the used butanone solvent has low price and easy reclaiming, and is applicable to industrial production.

Description

technical field [0001] The invention relates to a preparation method of a plant growth regulator, in particular to a preparation method of thiadizuron. Background technique [0002] Thidiazuron is a new type of high-efficiency plant growth regulator, its chemical name is 1-phenyl-3-(1,2,3-thiadiazol-5-yl)urea, its English name is Thidiazuron, referred to as TDZ. Its pure product is a colorless and odorless crystal with a melting point of 210.5-212.5°C (decomposition). Thidiazuron has strong cell division activity, can promote photosynthesis of plants, improve fruit quality, and increase fruit storability. Used as a shedding agent in cotton planting, after being absorbed by the leaves of the cotton plant, it can promote the natural formation of the separation tissue between the stalk and the stem as soon as possible, and the leaves will fall, which is beneficial to the mechanical harvesting of cotton, and can make cotton harvest About 10 days in advance, it helps to improv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D249/04A01P21/00
Inventor 孔繁蕾孙永辉王智敏史志兵
Owner 江苏省农用激素工程技术研究中心有限公司
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