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Method for preparing original medicne of 93% to 96% propargite

The technology of a special original drug, acetidine, is applied in the field of preparation of the original drug of acetidine with a content of 93% to 96%, which can solve the problems such as difficult removal of thionyl chloride, and achieve high content and high yield Effect

Active Publication Date: 2008-03-26
QINGDAO HANSEN BIOLOGIC SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The object of the present invention is to provide a kind of preparation method of the original drug of propargite with a content of 93% to 96%, which solves the problem that thionyl chloride is difficult to remove in the synthesis process of the original drug of propargite

Method used

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  • Method for preparing original medicne of 93% to 96% propargite
  • Method for preparing original medicne of 93% to 96% propargite
  • Method for preparing original medicne of 93% to 96% propargite

Examples

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Effect test

Embodiment 1

[0039] (1) Preparation of p-tert-butylphenoxycyclohexanol: in a 100L reactor, add 15.3Kg p-tert-butylphenol (98%, 100mol), 10.9Kg epoxycyclohexane (99%, 110mol) , toluene 32.24L (99%, 300mol), reacted at 120°C for 12 hours, washed three times, each time with 20Kg of hot water at a temperature of 70°C to 80°C; at a pressure of 15mmHg and a temperature of 115°C, vacuum distillation Excess epoxycyclohexane and toluene were removed in 2.5 hours to obtain 22.89 Kg of white p-tert-butylphenoxycyclohexanol, that is, the content of the first intermediate was 98.5%, and the yield was 99.0%.

[0040] (2) Preparation of 2-(4-tert-butyl) cyclohexyl chlorosulfite toluene solution: in a 50L reactor, 11.76Kg p-tert-butylphenoxycyclohexanol (98.5%, 50mol) was dissolved in 15L In toluene, when the temperature was lowered to 40° C., 5.95 Kg of thionyl chloride (99%, 50 mol) was added dropwise, and the mixture was kept at 35° C. for 15 hours. After the heat preservation is completed, add 1.81L ...

Embodiment 2

[0044](1) Preparation of p-tert-butylphenoxycyclohexanol: in a 100L reactor, add 15.3Kg p-tert-butylphenol (98%, 100mol), 10.9Kg epoxycyclohexane (99%, 110mol) , toluene 32.24L (99%, 300mol), reacted at 120°C for 12 hours, washed three times, each time with a temperature of 80°C hot water 20Kg; at a pressure of 25mmHg, a temperature of 120°C, decompression distillation for 3 hours Excessive epoxy cyclohexane and toluene were removed to obtain 22.89 Kg of white p-tert-butylphenoxycyclohexanol, that is, the content of the first intermediate was 98.5%, and the yield was 98.5%.

[0045] (2) Preparation of 2-(4-tert-butyl) cyclohexyl chlorosulfite toluene solution: in a 50L reactor, 11.76Kg p-tert-butylphenoxycyclohexanol (98.5%, 50mol) was dissolved in 15L In toluene, when the temperature was lowered to 40°C, 7.14Kg of thionyl chloride (99%, 60mol) was added dropwise, and the mixture was kept at 38°C for 13 hours. After the heat preservation is completed, 4.36L of dichloromethane...

Embodiment 3

[0049] Repeat the same steps as described in Example 1, but from step (2): the preparation of 2-(4-tert-butyl)cyclohexyl chlorosulfite toluene solution: in a 50L reactor, 11.76Kg Tert-butylphenoxycyclohexanol (98.5%, 50mol) was dissolved in 15L of toluene, and when the temperature was lowered to 40°C, 7.14Kg of thionyl chloride (99%, 60mol) was added dropwise, and kept at 38°C for 15 hours. After the heat preservation is completed, add 6.54L dichloroethane to the reaction kettle, and at 38°C, the pressure is 25mmHg, and the vacuum distillation is carried out for 4 hours to remove the excess thionyl chloride to obtain 2-(4-tert-butyl) The toluene solution of cyclohexyl chlorosulfite, that is, 48.5 mol of the second intermediate, has a yield of 97%.

[0050] The second intermediate is condensed with propynyl alcohol to obtain 93.6% of propargite content and 92.3% of propargite yield.

[0051] All the other are with embodiment 1.

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Abstract

A process for preparing high-purity propargite includes such steps as reaction between p-tert-butylphenol and 1,2-epoxy cyclohexane to generate p-tert-butylphenoxy cyclohexanol, reaction on sulfoxide chloride to generate 2-(4-tert-butyl) cyclohexylchlorine sulfite, adding low-boiling-point inertial solvent (petroether), removing excessive sulfoxide chloride in high vacuum degree, and condensation reaction on propynol.

Description

technical field [0001] The invention belongs to the technical field of pesticides containing a sulfur-oxygen double bond, and in particular relates to a method for preparing the original drug of propargite with a content of 93% to 96%. Background technique [0002] Propargite, also known as propargite, has a chemical name of 2-(4-tert-butylphenoxy)cyclohexylprop-2-ynyl sulfite, and is a highly efficient, low-toxic, broad-spectrum Acaricide, an acaricide with both contact and stomach poisoning effects, has remarkable efficacy and is not easy to produce drug resistance. It has been used in the world for more than 40 years and no problem of drug resistance has been found so far. It is mainly used for the control of mites in various economic crops such as citrus, apple, and cotton. my country's research on propargite began in the 1980s, and it was put into industrial production in the 1990s. Now there are more than a dozen domestic manufacturers with an annual output of about 2...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A01N41/02A01P7/02
Inventor 李树柏郭前玉刘瑞宾陈军汪农君吴凤
Owner QINGDAO HANSEN BIOLOGIC SCI
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