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Penconazole active compound and preparation method thereof

A technology of penconazole and original drug, which is applied in the field of penconazole original drug and its preparation, can solve the problems of high production of three wastes, low product content, difficult control of the production process of penconazole original drug, etc., and achieve the production of three wastes Less, resource-saving effect

Pending Publication Date: 2019-07-16
JIANGSU HEBEN BIOCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a kind of penconazole technical substance and preparation method thereof, solve the production process of penconazole technical substance to be difficult to control, the three wastes generation quantity is many, the product content is low etc. problem

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A kind of former drug of penconazole

[0030] The raw materials and parts by weight for preparing the original drug of penconazole are: 2,4-dichlorobutyrophenone 50g, dimethyl sulfoxide 40g, toluene 20g, dimethyl sulfate 30g, sodium hydroxide 25g, tetrabutyl bromide Ammonium chloride 1g, tetrahydrofuran 10g, zinc powder 12g, potassium carbonate 8g, 1,2,4-triazole 35g, methanesulfonyl chloride 20g, triethylamine 22g, methanol 15g, sodium methoxide 40g, cyclohexane 12g.

[0031] The preparation method of the former drug of penconazole, the steps are as follows:

[0032] Step S1, adding the parts by weight of toluene, 2,4-dichlorobutyrophenone, and dimethyl sulfoxide to the reactor, keeping the temperature at 25°C for 20 minutes, adding the parts by weight of dimethyl sulfate The temperature is kept at 25°C for 2 hours, the temperature is raised to 65°C for 3 hours, the temperature is lowered to 20°C and the weight of sodium hydroxide is added for 3 hours, the hydrochlori...

Embodiment 2

[0038] A kind of former drug of penconazole

[0039] The raw materials and parts by weight for preparing the original drug of penconazole are: 2,4-dichlorobutyrophenone 65g, dimethyl sulfoxide 50g, toluene 25g, dimethyl sulfate 35g, sodium hydroxide 30g, tetrabutyl bromide Ammonium chloride 2g, tetrahydrofuran 13g, zinc powder 13g, potassium carbonate 9g, 1,2,4-triazole 43g, methanesulfonyl chloride 30g, triethylamine 25g, methanol 18g, sodium methoxide 60g, cyclohexane 13g.

[0040] The preparation method of the former drug of penconazole, the steps are as follows:

[0041] Step S1, adding the parts by weight of toluene, 2,4-dichlorobutyrophenone, and dimethyl sulfoxide to the reactor, keeping the temperature at 28°C for 30 minutes, adding the parts by weight of dimethyl sulfate The temperature is kept at 25°C for 2.5h, the temperature is raised to 65°C for 3h, the temperature is lowered to 20°C and the weight of sodium hydroxide is added for 3h, and the hydrochloric acid is n...

Embodiment 3

[0047] A kind of former drug of penconazole

[0048] The raw materials and parts by weight for preparing the original drug of penconazole are: 2,4-dichlorobutyrophenone 80g, dimethyl sulfoxide 60g, toluene 30g, dimethyl sulfate 40g, sodium hydroxide 30g, tetrabutyl bromide Ammonium chloride 2g, tetrahydrofuran 15g, zinc powder 15g, potassium carbonate 10g, 1,2,4-triazole 47g, methanesulfonyl chloride 40g, triethylamine 28g, methanol 20g, sodium methoxide 80g, cyclohexane 14g.

[0049] The preparation method of the former drug of penconazole, the steps are as follows:

[0050] Step S1, adding the parts by weight of toluene, 2,4-dichlorobutyrophenone, and dimethyl sulfoxide to the reactor, keeping the temperature at 30°C for 40 minutes, adding the parts by weight of dimethyl sulfate The temperature is kept at 25°C for 2.5h, the temperature is raised to 75°C for 3h, the temperature is lowered to 20°C and the weight of sodium hydroxide is added for 3h, and the hydrochloric acid i...

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Abstract

The invention provides a penconazole active compound and a preparation method thereof. The raw materials comprise, in parts by weight, 50-80 parts of 2,4-dichlorobutyrophenone, 40-60 parts of dimethylsulfoxide, 20-30 parts of toluene, 30-40 parts of dimethyl sulfate, 25-30 parts of sodium hydroxide, 1-2 parts of tetrabutylammonium bromide, 10-15 parts of tetrahydrofuran, 12-15 parts of zinc powder, 8-10 parts of potassium carbonate, 35-47 parts of 1,2,4-triazole, 20-40 parts of methylsulfonyl chloride, 22-28 parts of triethylamine, 15-20 parts of methanol, 40-80 parts of sodium methoxide and12-14 parts of cyclohexane. After application of the prepared penconazole active compound to powdery mildew of pumpkin, grapes, nuts, vegetables and other crops, a good curative effect and a long-lasting effect are achieved, and the efficacy is higher than that of congeneric products.

Description

technical field [0001] The invention relates to the technical field of penconazole, in particular to a technical field of penconazole and a preparation method thereof. Background technique [0002] Penconazole is a high-efficiency and low-toxic fungicide developed by Ciba-Geigy Corporation. Its chemical name is 1-(2,4-dichloro--propylphenethyl)-1H-1,2,4-triazine Azole, common name penconazole. Appearance is colorless crystalline powder, melting point 57.6-60.3°C; vapor pressure: 0.017mPa (20°C), 0.37mPa (25°C); KowLogP=3.72 (H5.7, 25°C); solubility: 73mg / L in water (25°C) ℃); in organic solvents (g / L, 25℃): 730 in ethanol, 770 in acetone, 610 in toluene, 24 in n-hexane, 400 in n-octanol; stability: stable in water, stable up to 350℃ , not decomposed. It is a systemic triazole fungicide with protective, therapeutic and eradicating effects, with a dosage of 10~50gai / hm 2 Dosage, can control the pathogenic bacteria of powdery mildew family, black star fungus and other patho...

Claims

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Application Information

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IPC IPC(8): C07D249/08
CPCC07D249/08
Inventor 陈华曾挺潘光飞
Owner JIANGSU HEBEN BIOCHEM
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