CN107383089A - A kind of new technology for synthesizing fenifrothion - Google Patents

A kind of new technology for synthesizing fenifrothion Download PDF

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Publication number
CN107383089A
CN107383089A CN201710505541.3A CN201710505541A CN107383089A CN 107383089 A CN107383089 A CN 107383089A CN 201710505541 A CN201710505541 A CN 201710505541A CN 107383089 A CN107383089 A CN 107383089A
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CN
China
Prior art keywords
fenifrothion
reaction
metacresol
compound
new technology
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710505541.3A
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Chinese (zh)
Inventor
刘伟
李惠跃
张彦祥
王洪东
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Lianyungang Avilive Chemical Co Ltd
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Lianyungang Avilive Chemical Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by Lianyungang Avilive Chemical Co Ltd filed Critical Lianyungang Avilive Chemical Co Ltd
Priority to CN201710505541.3A priority Critical patent/CN107383089A/en
Publication of CN107383089A publication Critical patent/CN107383089A/en
Pending legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F9/00Compounds containing elements of Groups 5 or 15 of the Periodic System
    • C07F9/02Phosphorus compounds
    • C07F9/06Phosphorus compounds without P—C bonds
    • C07F9/16Esters of thiophosphoric acids or thiophosphorous acids
    • C07F9/165Esters of thiophosphoric acids
    • C07F9/18Esters of thiophosphoric acids with hydroxyaryl compounds

Abstract

A kind of new technology for synthesizing fenifrothion, including (1) condensation reaction:By metacresol (compound one) and alkali reaction generation metacresol salt, alkali is one or more combinations in sodium hydroxide, sodium carbonate, potassium hydroxide and potassium carbonate, metacresol salt generates condensation product with Methochloride under the conditions of existing for catalyst, catalyst is the mantoquita of monovalence, comprising being not limited solely to stannous chloride, cuprous bromide, cuprous oxide;(2) nitration reaction:Condensation product and nitric acid reaction generation target product fenifrothion will be made in step (1), the temperature of nitration reaction is 10 50 DEG C;It is an advantage of the invention that the method have the advantages that the concise in technology easily produces, obtained fenifrothion mass fraction >=96&, side reaction is seldom, is adapted to large-scale industrial production, pollutes small, energy-conserving and environment-protective.

Description

A kind of new technology for synthesizing fenifrothion
Technical field
The present invention relates to chemical technology field, and in particular to a kind of new technology for synthesizing fenifrothion.
Background technology
Fenifrothion is a kind of broad-spectrum organic insecticide of efficiently low residual hazard, has infiltration systemic action, therefore it There are good prevention effect, such as snout moth's larva of rice, rice winged insect, cotton red sandfly insect, eating-core bean worm, aphid to the insect of various crop And fruit tree, Pests of Tea-Plants are also effective to mosquitos and flies etc.;The conventional method of the compound is synthesized mainly using metacresol as raw material, Nitration reaction is first carried out, then carries out condensation reaction.
Nitrifying main reaction equation is:
Following side reaction also be present in nitrification:
Above side reaction is all relevant with phenolic hydroxyl group, causes side reaction excessive, and economically unreasonable, content does not reach.
The content of the invention
In order to solve the above technical problems, the present invention adopts the following technical scheme that:
A kind of new technology for synthesizing fenifrothion, including:
(1) condensation reaction:Metacresol (compound one) and Methochloride (compound two) reaction generation intermediate condensation Thing (compound three);
(2) nitration reaction:Condensation product (compound three) and nitric acid reaction generation target product fenifrothion.
Preferably, in the condensation reaction, the step of metacresol reacts with Methochloride (compound two), is as follows:
1) by metacresol (compound one) and alkali reaction generation metacresol salt;
2) metacresol salt and Methochloride are generated into condensation product (compound three) under the conditions of existing for catalyst.
Preferably, the alkali is one or more combinations in sodium hydroxide, sodium carbonate, potassium hydroxide and potassium carbonate.
Preferably, the catalyst is the mantoquita of monovalence, sub- comprising stannous chloride, cuprous bromide, oxidation is not limited solely to Copper.
Preferably, the temperature of nitration reaction is 10-50 DEG C.
The method have the advantages that:The concise in technology easily produces, and fenifrothion mass fraction >=96& is made, and side reaction is seldom, fits Large-scale industrial production is closed, pollutes small, energy-conserving and environment-protective.
Embodiment
A kind of new technology for synthesizing fenifrothion, including:
(1) condensation reaction:By metacresol (compound one) and alkali reaction generation metacresol salt, alkali is sodium hydroxide, carbonic acid One or more combinations in sodium, potassium hydroxide and potassium carbonate, metacresol salt is with Methochloride in condition existing for catalyst Lower generation condensation product, catalyst is the mantoquita of monovalence, comprising being not limited solely to stannous chloride, cuprous bromide, cuprous oxide;
(2) nitration reaction:Condensation product and nitric acid reaction generation target product fenifrothion, nitrification will be made in step (1) The temperature of reaction is 10-50 DEG C.
Illustrate the implementation of the technical program with specific embodiment below.
Embodiment one:
A kind of new technology for synthesizing fenifrothion, including:
(1) condensation reaction:By metacresol (compound one) and sodium hydroxide reaction generation metacresol salt, metacresol salt and first Base chloride generates condensation product under the conditions of existing for catalyst stannous chloride;
(2) nitration reaction:Condensation product and nitric acid reaction generation target product fenifrothion, nitrification will be made in step (1) The temperature of reaction is 10 DEG C.
Embodiment two:
A kind of new technology for synthesizing fenifrothion, including:
(1) condensation reaction:By metacresol (compound one) and sodium carbonate reaction generation metacresol salt, metacresol salt and methyl Chloride generates condensation product under the conditions of existing for catalyst cuprous bromide;
(2) nitration reaction:Condensation product and nitric acid reaction generation target product fenifrothion, nitrification will be made in step (1) The temperature of reaction is 30 DEG C.
Embodiment three:
A kind of new technology for synthesizing fenifrothion, including:
(1) condensation reaction:By metacresol (compound one) and potassium hydroxide reaction generation metacresol salt, metacresol salt and first Base chloride generates condensation product under the conditions of existing for catalyst cuprous oxide;
(2) nitration reaction:Condensation product and nitric acid reaction generation target product fenifrothion, nitrification will be made in step (1) The temperature of reaction is 50 DEG C.
It is upper described, it is only the embodiment of the present invention, but protection scope of the present invention is not limited thereto, and it is any ripe Know those skilled in the art the invention discloses technical scope in, change or replacement can be readily occurred in, should all be covered Within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.

Claims (5)

  1. A kind of 1. new technology for synthesizing fenifrothion, it is characterised in that including:
    (1) condensation reaction:Metacresol (compound one) and Methochloride (compound two) reaction generation
    (2) nitration reaction:Condensation product (compound three) and nitric acid reaction generation target product fenifrothion.
  2. A kind of 2. new technology for synthesizing fenifrothion according to claim 1, it is characterised in that:In the condensation reaction, The step of metacresol reacts with Methochloride (compound two) is as follows:
    1) by metacresol (compound one) and alkali reaction generation metacresol salt;
    2) metacresol salt and Methochloride are generated into condensation product (compound three) under the conditions of existing for catalyst.
  3. 3. according to a kind of new technology of synthesis fenifrothion described in claim 2, it is characterised in that:The alkali is hydroxide One or more combinations in sodium, sodium carbonate, potassium hydroxide and potassium carbonate.
  4. 4. according to a kind of new technology of synthesis fenifrothion described in claim 2, it is characterised in that:The catalyst is monovalence Mantoquita, comprising being not limited solely to stannous chloride, cuprous bromide, cuprous oxide.
  5. 5. according to a kind of new technology of synthesis fenifrothion described in claim 1, it is characterised in that:The temperature of nitration reaction is 10-50℃。
CN201710505541.3A 2017-06-28 2017-06-28 A kind of new technology for synthesizing fenifrothion Pending CN107383089A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710505541.3A CN107383089A (en) 2017-06-28 2017-06-28 A kind of new technology for synthesizing fenifrothion

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710505541.3A CN107383089A (en) 2017-06-28 2017-06-28 A kind of new technology for synthesizing fenifrothion

Publications (1)

Publication Number Publication Date
CN107383089A true CN107383089A (en) 2017-11-24

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710505541.3A Pending CN107383089A (en) 2017-06-28 2017-06-28 A kind of new technology for synthesizing fenifrothion

Country Status (1)

Country Link
CN (1) CN107383089A (en)

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2318116A (en) * 1996-10-10 1998-04-15 Zeneca Ltd Nitration of Diphenoxy compounds

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2318116A (en) * 1996-10-10 1998-04-15 Zeneca Ltd Nitration of Diphenoxy compounds

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
NISHIZAWA YOSHIHIKO等: "Studies on the Organophosphorus Insecticides", 《AGR. BIOL. CHEM.》 *
王元正: "从混合间对甲酚制备杀螟硫磷", 《应用化学》 *

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Application publication date: 20171124