CN107266358A - A kind of Nylar active compound synthetic method - Google Patents
A kind of Nylar active compound synthetic method Download PDFInfo
- Publication number
- CN107266358A CN107266358A CN201710472530.XA CN201710472530A CN107266358A CN 107266358 A CN107266358 A CN 107266358A CN 201710472530 A CN201710472530 A CN 201710472530A CN 107266358 A CN107266358 A CN 107266358A
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- CN
- China
- Prior art keywords
- nylar
- pop
- active compound
- synthetic method
- ppp
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- 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.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D213/62—Oxygen or sulfur atoms
- C07D213/63—One oxygen atom
- C07D213/64—One oxygen atom attached in position 2 or 6
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Pyridine Compounds (AREA)
Abstract
The invention discloses a kind of Nylar active compound synthetic method, comprise the following steps：POP is synthesized：Phenol switchs to POP with parachlorophenol reaction, and self-polymeric reaction can occur for phenol and parachlorophenol in addition, switch to Biphenyl Ether and 4,4 dichlorobenzene ethers；PPP is synthesized：With expoxy propane condensation reaction occurs for POP, switchs to PPP；Nylar is synthesized：Condensation reaction occurs for PPP and 2 chloropyridines, potassium hydroxide, switchs to Nylar.The POP is 4 xenol ethers.It is an advantage of the invention that：React yield high, substantially increase production efficiency, reaction raw materials used are moderate and environmentally safe.
Description
Technical field
The present invention relates to pesticide field, and in particular to a kind of Nylar active compound synthetic method.
Background technology
Nylar (pyriproxyfen), also known as go out young precious, pyriproxyfen, and chemical name is 4- phenoxy phenyls-(RS) -2-
(2- pyridine radicals oxygen) propyl ether, is in the one of nineteen eighty-three initiative exploitation by SUMITOMO CHEMICAL (Sumitomo Chemical) company
Class alcoxyl pyridine juvenile hormone class chitin synthesis inhibitor, realizes commercialization in 1991.
The main formulation of Nylar has granule, missible oil, suspending agent and with agent, is widely used in water fruits and vegetables, cotton
With the preventing and treating of trialeurodes vaporariorum on ornamental plant and scale insect, and mosquitos and flies control and animal health in public health.Its photostability
Good, consumption is few, and activity is high, and blade conductibility inhales strong with interior, and the lasting period is long, to crop safety, to mammal low toxicity and to life
State ambient influnence is small, meets the target of human ecological environment protection, it is considered to be one of effective means of integrated pest management, into
For a key areas of insecticide research and development.
The content of the invention
The invention provides a kind of Nylar active compound synthetic method, step is simplified, simple and easy to apply.
The technical solution adopted by the present invention is：
A kind of Nylar active compound synthetic method, comprises the following steps：
A, POP are synthesized：Phenol switchs to POP with parachlorophenol reaction, and self-polymeric reaction can occur for phenol and parachlorophenol in addition,
Switch to Biphenyl Ether and 4,4- dichlorobenzene ethers；
B, PPP are synthesized：With expoxy propane condensation reaction occurs for POP, switchs to PPP；
C, Nylar synthesis：With 2- chloropyridines, potassium hydroxide condensation reaction occurs for PPP, switchs to Nylar.
Further, the reaction yield about 92% of the step a, the reaction yield about 97.5% of the step b, the step
C reaction yield about 97.8%.
Further, the POP is 4- xenol ethers.
Further, the equipment such as washing kettle, reactor and distillation still are needed in the new technology implementation process.
The beneficial effects of the invention are as follows：React yield high, substantially increase production efficiency, reaction raw materials price used is fitted
In, and it is environmentally safe.
Embodiment
In order to deepen the understanding of the present invention, below in conjunction with embodiment, the invention will be further described, the embodiment
It is only used for explaining the present invention, is not intended to limit the scope of the present invention..
A kind of Nylar active compound synthetic method, its specific implementation step is as follows：
1. POP is synthesized：By in a certain amount of phenol, potassium hydroxide, toluene input reactor, azeotropic removes the moisture content in raw material,
After freezing is reclaimed, condensate liquid makees waste water through fraction water device water-dividing, toluene layer reuse, water.
Parachlorophenol is slowly added dropwise in reactor, 180 DEG C of temperature in the kettle is controlled, reacts 10 hours., will after the completion of reaction
Material is all transferred in washing kettle, plus salt acid for adjusting pH is to 3-4, reheats water washing, after washing, is transferred to distillation still and is depressurized
Distillation, front-end volatiles are mainly unreacted phenol etc., are back to dehydration procedure, and midbarrel is POP, collect stand-by, kettle is residual to be consolidated
It is useless.
Stannous chloride class catalyst is used in POP synthesis, solid-state, consumption is about 0.1t, enter residual in vacuum distillation workshop section
Slag.
2. PPP is synthesized：It will be stirred in a certain amount of water, sodium hydroxide, POP input reactors, epoxy third be added dropwise under normal temperature
Alkane, is dripped, and is gradually heating to 70 DEG C, insulation reaction a few hours, is added salt acid for adjusting pH to 5-7 after the completion of reaction, be then centrifuged for
It is stand-by after dehydration, drying.
3. Nylar is synthesized：A certain amount of PPP, toluene, potassium hydroxide are added in reactor, then reflux dewatering drops
2- chloropyridines are added dropwise to 50-70 DEG C in temperature, are added dropwise to complete rear temperature rising reflux reaction a few hours, after question response is complete, the washing that adds water is removed
Salt, then depressurizes precipitation and steams toluene and apply mechanically, after the completion of precipitation again plus methanol dissolving, recrystallization, through filtering, dries, after drying
Obtain Nylar active compound.The methanol distillation reuse filtered out, kettle is residual to make solid waste.
Claims (4)
1. a kind of Nylar active compound synthetic method, it is characterised in that comprise the following steps：
A, POP are synthesized：Phenol switchs to POP with parachlorophenol reaction, and self-polymeric reaction can occur for phenol and parachlorophenol in addition,
Switch to Biphenyl Ether and 4,4- dichlorobenzene ethers；
B, PPP are synthesized：With expoxy propane condensation reaction occurs for POP, switchs to PPP；
C, Nylar synthesis：With 2- chloropyridines, potassium hydroxide condensation reaction occurs for PPP, switchs to Nylar.
2. a kind of Nylar active compound synthetic method according to claim 1, it is characterised in that the step a's reacts
Rate about 92%, the reaction yield about 97.5% of the step b, the reaction yield about 97.8% of the step c.
3. a kind of Nylar active compound synthetic method according to claim 1, it is characterised in that the POP joins for 4- hydroxyls
Phenylate.
4. a kind of Nylar active compound synthetic method according to claim 1, it is characterised in that the new technology implementation process
In need the equipment such as washing kettle, reactor and distillation still.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710472530.XA CN107266358A (en) | 2017-06-21 | 2017-06-21 | A kind of Nylar active compound synthetic method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710472530.XA CN107266358A (en) | 2017-06-21 | 2017-06-21 | A kind of Nylar active compound synthetic method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107266358A true CN107266358A (en) | 2017-10-20 |
Family
ID=60067842
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710472530.XA Pending CN107266358A (en) | 2017-06-21 | 2017-06-21 | A kind of Nylar active compound synthetic method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107266358A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107311922A (en) * | 2017-09-05 | 2017-11-03 | 南通派斯第农药化工股份有限公司 | A kind of synthetic method of third pyrrole ether |
| CN108383807A (en) * | 2018-04-12 | 2018-08-10 | 深圳市前海博扬研究院有限公司 | A method of reducing the discharge of etherification reaction brine waste |
| CN110372581A (en) * | 2019-08-19 | 2019-10-25 | 南通嘉禾化工有限公司 | A method of preparing 2-(3- 4-trifluoromethylphenopendant) -6- trichloromethyl pyridine |
-
2017
- 2017-06-21 CN CN201710472530.XA patent/CN107266358A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107311922A (en) * | 2017-09-05 | 2017-11-03 | 南通派斯第农药化工股份有限公司 | A kind of synthetic method of third pyrrole ether |
| CN108383807A (en) * | 2018-04-12 | 2018-08-10 | 深圳市前海博扬研究院有限公司 | A method of reducing the discharge of etherification reaction brine waste |
| CN108383807B (en) * | 2018-04-12 | 2020-10-27 | 深圳市前海博扬研究院有限公司 | Method for reducing discharge of salt-containing wastewater of etherification reaction |
| CN110372581A (en) * | 2019-08-19 | 2019-10-25 | 南通嘉禾化工有限公司 | A method of preparing 2-(3- 4-trifluoromethylphenopendant) -6- trichloromethyl pyridine |
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| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
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Application publication date: 20171020 |