A kind of method of synthesizing blastamide

A technology of blastamide and toluene, applied in the field of synthesizing blastamide, can solve problems such as unfavorable popularization and application, long reaction time, complex process, etc., and achieve the effects of reducing raw material types, shortening reaction cycle, and simplifying the process route

Active Publication Date: 2016-05-25
JINGBO AGROCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process is complicated, the reaction time is long, and acid gases such as sulfur dioxide and hydrogen chloride will be produced, which will corrode equipment and pollute the air, which is not conducive to popularization and application.

Method used

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  • A kind of method of synthesizing blastamide

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Experimental program
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Effect test

Embodiment 1

[0018] 163g (1mol) of 2,4-dichlorophenol, 1L of toluene, 40g (1mol) of sodium hydroxide and 122.5g (1mol) of methyl 2-chloropropionate were added to the 2L reaction flask, and the temperature was raised to 55°C for reaction 8 Hour, the toluene phase is washed with water after the reaction is finished, and the toluene phase after the washing is carried out to distill the solvent under reduced pressure to obtain methyl propionate;

[0019] 112g (1mol) of 2-amino-2,3-dimethylbutyronitrile, 550ml of toluene and 84g (1mol) of sodium bicarbonate and the methyl propionate obtained by the reaction were added to the 1L reaction flask, and the temperature was controlled at 15°C to carry out The reaction was carried out for 6 hours, the toluene phase was washed with water after the reaction, and the toluene phase after the washing was carried out to distill the solvent under reduced pressure, and then recrystallized with a mixed solvent of 1.1 L of water and ethanol, and the volume ratio ...

Embodiment 2

[0021] 163g (1mol) of 2,4-dichlorophenol, 1.2L of toluene, 40g (1mol) of sodium hydroxide and 134.8g (1.1mol) of methyl 2-chloropropionate were added to a 2L reaction flask, and the temperature was raised to 60°C The reaction was carried out for 9 hours, the toluene phase was washed with water after the reaction, and the toluene phase after the washing was carried out under reduced pressure distillation solvent to obtain methyl propionate;

[0022] 112g (1mol) of 2-amino-2,3-dimethylbutyronitrile, 500ml of toluene and 84g (1mol) of sodium bicarbonate and methyl propionate obtained by the reaction were added to the 1L reaction flask, and the temperature was controlled at 10°C to carry out The reaction was carried out for 5 hours, and the toluene phase was washed with water after the reaction, and the toluene phase after the washing was carried out to distill the solvent under reduced pressure, and then recrystallized with a mixed solvent of 1 L of water and ethanol, and the volu...

Embodiment 3

[0024] 163g (1mol) of 2,4-dichlorophenol, 1.3L of toluene, 40g (1mol) of sodium hydroxide and 147g (1.2mol) of methyl 2-chloropropionate were added to the 2L reaction flask, and the temperature was raised to 45°C for reaction For 10 hours, the toluene phase was washed with water after the reaction, and the toluene phase after the water washing was subjected to reduced pressure distillation of the solvent to obtain methyl propionate;

[0025] Add 112g (1mol) of 2-amino-2,3-dimethylbutyronitrile, 550ml of toluene and 84g (1mol) of sodium bicarbonate and the methyl propionate obtained by the reaction to the 1L reaction flask, and the temperature is controlled at 8°C to carry out The reaction was carried out for 7 hours, and the toluene phase was washed with water after the reaction, and the toluene phase after the washing was carried out to distill the solvent under reduced pressure, and then recrystallized with a mixed solvent of 1.2 L of water and ethanol. The volume ratio of th...

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Abstract

The invention relates to a novel method for synthesizing fenoxanil serving as a systemic fungicide. The novel method for synthesizing fenoxanil serving as the systemic fungicide comprises the following steps: adding 2,4-dichlorophenol, sodium hydroxide and 2-methyl chloropropionate into a methyl benzene solvent, controlling reaction temperature at 30-70 DEG C, washing methyl benzene phase by using water after the reaction is ended, and carrying out reduced pressure distillation on a solvent of the washed methyl benzene phase to obtain dichlorprop methyl ester; and adding the obtained dichlorprop methyl ester into a methyl benzene solution with dissolved 2-amino-2,3-dimethyl butyronitrile and sodium bicarbonate, reacting by controlling the reaction temperature at 0-30 DEG C, washing the methyl benzene phase by using water after the reaction is ended, carrying out reduced pressure distillation on a solvent of the washed methyl benzene phase, recrystallizing by using a mixed solvent of water and ethyl alcohol, reducing the temperature to the room temperature, and filtering to obtain the fenoxanil. According to the synthesis method, 2-chloropropionic acid is replaced by 2-methyl chloropropionate; dipropionyl chloride is replaced by the generated dichlorprop methyl ester; one-step acylation reaction is eliminated; the process route is simplified; the reaction period is shortened; the method has great development in the industrial production.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a new method for synthesizing rice blast amide. Background technique [0002] Rice blast amide, also known as cyanobactam, is a novel systemic fungicide for the control of rice blast, widely used in rice sheath blight, rice blast and rice bacterial blight. The existing synthetic method of the product adopts the reaction of 2-chloropropionic acid and 2,4-dichlorophenol to generate dropwise propionic acid chloride. There are also bibliographical reports, in the mixed system of the toluene liquid that is dissolved with 2-amino-2,3-dimethylbutyronitrile and the aqueous solution that is dissolved with sodium bicarbonate, add the toluene liquid of propionic acid chloride, keep the reaction in the ice-water bath. conditions to produce blastamide. The process is complicated, the reaction time is long, and acid gas sulfur dioxide and hydrogen chloride are also produced, whic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/29C07C253/30
Inventor 马文娟韦能春曹同波戴荣华王宗逄廷超王清新
Owner JINGBO AGROCHEM TECH CO LTD
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