CN109232307A - A kind of purification process of tralkoxydim - Google Patents
A kind of purification process of tralkoxydim Download PDFInfo
- Publication number
- CN109232307A CN109232307A CN201811241939.1A CN201811241939A CN109232307A CN 109232307 A CN109232307 A CN 109232307A CN 201811241939 A CN201811241939 A CN 201811241939A CN 109232307 A CN109232307 A CN 109232307A
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- CN
- China
- Prior art keywords
- tralkoxydim
- filtrate
- purification process
- filters
- triethanolamine
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C249/00—Preparation of compounds containing nitrogen atoms doubly-bound to a carbon skeleton
- C07C249/04—Preparation of compounds containing nitrogen atoms doubly-bound to a carbon skeleton of oximes
- C07C249/14—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/16—Systems containing only non-condensed rings with a six-membered ring the ring being unsaturated
Abstract
The invention belongs to organic compound technical field of purification, in particular to a kind of purification process of tralkoxydim includes the following steps, step 1, by tralkoxydim crude product dissolve by heating in glycol dimethyl ether, triethanolamine, ethyl acetate mixed solution in；Step 2, it filters while hot, removes insoluble matter, take filtrate；Step 3, hexane is added in the filtrate obtained to step 2, after continuing heating stirring, removes half solvent, filters while hot, remove insoluble matter, take filtrate；Step 4, filtrate step 3 obtained is cooled to 10-20 DEG C, filters, takes filter cake, as tralkoxydim sterling；The purification process of tralkoxydim of the invention uses the mixed solution of glycol dimethyl ether, triethanolamine, ethyl acetate for the solvent of recrystallization, so that tralkoxydim crude product can be dissolved at 80-90 DEG C, and remove impurity, it adds hexane and removes half solvent, remove residual impurity, solubility is adjusted, the tralkoxydim that purity is up to 99.9% is made after cooling.
Description
Technical field
The invention belongs to organic compound technical field of purification, in particular to a kind of purification process of tralkoxydim.
Background technique
Tralkoxydim is for white tasteless crystalline solid, and chemical name is 2- (l- (ethoxy imino) propyl) -3- hydroxyl -5-
(2,4,6- trimethylphenyl) cyclohexene -2- ketone, also known as methoxyphenone, can effectively prevent and kill off a variety of gramineae weeds of wheatland, wherein wrapping
Wild avena sativa is included, is a kind of highly selective herbicide.
By 2,4,6- trimethyl formaldehyde and condensation of acetone, obtained beta-unsaturated ketone is reacted with diethyl malonate；Product
Through hydrolysis, cyclisation, decarboxylation, 3- hydroxyl -5- (2,4,6- trimethylphenyl)-hexamethylene -2- alkene 1- ketone is obtained, the compound is in methanol
In the presence of sodium, with propionic acid anhydride reactant, 3- hydroxyl -5- (2,4,6- trimethylphenyl) -2- propiono-hexamethylene -2- alkene -1- is obtained
Ketone；It is finally reacted again with ethoxy amine hydrochloride to get tralkoxydim crude product, tralkoxydim crude product can obtain tralkoxydim sterling by purifying；
But the tralkoxydim sterling that existing conventional purification method obtains is not high, and only 95% or so.
Summary of the invention
The present invention solves the above-mentioned technical problems in the prior art, provides a kind of purification process of tralkoxydim.
To solve the above problems, technical scheme is as follows:
A kind of purification process of tralkoxydim, includes the following steps,
Step 1, by tralkoxydim crude product dissolve by heating in glycol dimethyl ether, triethanolamine, ethyl acetate mixed solution
In；
Step 2, it filters while hot, removes insoluble matter, take filtrate；
Step 3, hexane is added in the filtrate obtained to step 2, after continuing heating stirring, removes half solvent, while hot mistake
Filter removes insoluble matter, takes filtrate；
Step 4, filtrate step 3 obtained is cooled to 10-20 DEG C, filters, takes filter cake, as tralkoxydim sterling.
Preferably, in the mixed solution of the glycol dimethyl ether, triethanolamine, ethyl acetate, glycol dimethyl ether, three
Ethanol amine, ethyl acetate volume ratio be 2-4:2:1.
Preferably, the heating for dissolving temperature of the step 1 is 80-90 DEG C.
Preferably, in the step 3, the volume ratio of the filtrate and hexane is 1:0.8-1.
Preferably, in the step 4, cooling time 30-40min.
Compared with the existing technology, advantages of the present invention is as follows,
The purification process of tralkoxydim of the invention uses the mixed solution of glycol dimethyl ether, triethanolamine, ethyl acetate
For the solvent of recrystallization, so that tralkoxydim crude product can be dissolved at 80-90 DEG C, and impurity is removed, it is semi-soluble to add hexane removing one
Agent removes residual impurity, adjusts solubility, the tralkoxydim that purity is up to 99.9% is made after cooling.
Specific embodiment
Embodiment 1:
A kind of purification process of tralkoxydim, includes the following steps,
Step 1, tralkoxydim crude product is dissolved by heating in volume ratio is 2:2:1 glycol dimethyl ether, triethanolamine, acetic acid second
In the mixed solution of ester；Dissolving by heating temperature is 80-90 DEG C；
Step 2, it filters while hot, removes insoluble matter, take filtrate；
Step 3, hexane is added in the filtrate obtained to step 2, and the volume ratio of the filtrate and hexane is 1:0.8；Continue
After heating stirring, half solvent is removed, is filtered while hot, removed insoluble matter, take filtrate；
Step 4, the filtrate that step 3 obtains is cooled to 10-20 DEG C in 30-40min, filters, takes filter cake, as tralkoxydim
Sterling, purity 99.8%.
Embodiment 2:
A kind of purification process of tralkoxydim, includes the following steps,
Step 1, tralkoxydim crude product is dissolved by heating in volume ratio is 3:2:1 glycol dimethyl ether, triethanolamine, acetic acid second
In the mixed solution of ester；Dissolving by heating temperature is 80-90 DEG C；
Step 2, it filters while hot, removes insoluble matter, take filtrate；
Step 3, hexane is added in the filtrate obtained to step 2, and the volume ratio of the filtrate and hexane is 1:0.9；Continue
After heating stirring, half solvent is removed, is filtered while hot, removed insoluble matter, take filtrate；
Step 4, the filtrate that step 3 obtains is cooled to 10-20 DEG C in 30-40min, filters, takes filter cake, as tralkoxydim
Sterling, purity 99.9%.
Embodiment 3:
A kind of purification process of tralkoxydim, includes the following steps,
Step 1, tralkoxydim crude product is dissolved by heating in volume ratio is 4:2:1 glycol dimethyl ether, triethanolamine, acetic acid second
In the mixed solution of ester；Dissolving by heating temperature is 80-90 DEG C；
Step 2, it filters while hot, removes insoluble matter, take filtrate；
Step 3, hexane is added in the filtrate obtained to step 2, and the volume ratio of the filtrate and hexane is 1:1；Continue to add
After thermal agitation, half solvent is removed, is filtered while hot, removed insoluble matter, take filtrate；
Step 4, the filtrate that step 3 obtains is cooled to 10-20 DEG C in 30-40min, filters, takes filter cake, as tralkoxydim
Sterling, purity 99.8%.
It should be noted that above-described embodiment is only presently preferred embodiments of the present invention, there is no for the purpose of limiting the invention
Protection scope, the equivalent substitution or substitution made on the basis of the above all belong to the scope of protection of the present invention.
Claims (5)
1. a kind of purification process of tralkoxydim, which is characterized in that include the following steps,
Step 1, by tralkoxydim crude product dissolve by heating in glycol dimethyl ether, triethanolamine, ethyl acetate mixed solution in；
Step 2, it filters while hot, removes insoluble matter, take filtrate；
Step 3, hexane is added in the filtrate obtained to step 2, after continuing heating stirring, removes half solvent, filters, remove while hot
Insoluble matter is removed, filtrate is taken；
Step 4, filtrate step 3 obtained is cooled to 10-20 DEG C, filters, takes filter cake, as tralkoxydim sterling.
2. the purification process of tralkoxydim as described in claim 1, which is characterized in that the glycol dimethyl ether, triethanolamine,
In the mixed solution of ethyl acetate, glycol dimethyl ether, triethanolamine, ethyl acetate volume ratio be 2-4:2:1.
3. the purification process of tralkoxydim as described in claim 1, which is characterized in that the heating for dissolving temperature of the step 1 is
80-90℃。
4. the purification process of tralkoxydim as described in claim 1, which is characterized in that in the step 3, the filtrate and hexane
Volume ratio be 1:0.8-1.
5. the purification process of tralkoxydim as described in claim 1, which is characterized in that in the step 4, cooling time 30-
40min。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811241939.1A CN109232307A (en) | 2018-10-24 | 2018-10-24 | A kind of purification process of tralkoxydim |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811241939.1A CN109232307A (en) | 2018-10-24 | 2018-10-24 | A kind of purification process of tralkoxydim |
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| Publication Number | Publication Date |
|---|---|
| CN109232307A true CN109232307A (en) | 2019-01-18 |
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|---|---|---|---|
| CN201811241939.1A Pending CN109232307A (en) | 2018-10-24 | 2018-10-24 | A kind of purification process of tralkoxydim |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0080301A2 (en) * | 1981-11-20 | 1983-06-01 | Ici Australia Limited | Herbicidal cyclohexane-1,3-dione derivatives |
| US4482740A (en) * | 1981-12-29 | 1984-11-13 | Nippon Soda Company Limited | 5-Phenylcyclohexenone derivatives |
| CN1207090A (en) * | 1995-12-05 | 1999-02-03 | 巴斯福股份公司 | Cyclohexenone oxime ether metal salts |
| CN101427679A (en) * | 2007-11-07 | 2009-05-13 | 沈阳朗农科技有限公司 | Oxime ether-derivative herbicides and uses thereof |
-
2018
- 2018-10-24 CN CN201811241939.1A patent/CN109232307A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0080301A2 (en) * | 1981-11-20 | 1983-06-01 | Ici Australia Limited | Herbicidal cyclohexane-1,3-dione derivatives |
| US4760192A (en) * | 1981-11-20 | 1988-07-26 | Imperial Chemical Industries Plc | Herbicidal cyclohexane-1,3-dione derivatives |
| US4482740A (en) * | 1981-12-29 | 1984-11-13 | Nippon Soda Company Limited | 5-Phenylcyclohexenone derivatives |
| CN1207090A (en) * | 1995-12-05 | 1999-02-03 | 巴斯福股份公司 | Cyclohexenone oxime ether metal salts |
| CN101427679A (en) * | 2007-11-07 | 2009-05-13 | 沈阳朗农科技有限公司 | Oxime ether-derivative herbicides and uses thereof |
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Effective date of abandoning: 20230818 |
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