CN114702502A - Method for refining triazole pyrimidone - Google Patents
Method for refining triazole pyrimidone Download PDFInfo
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- CN114702502A CN114702502A CN202210545817.1A CN202210545817A CN114702502A CN 114702502 A CN114702502 A CN 114702502A CN 202210545817 A CN202210545817 A CN 202210545817A CN 114702502 A CN114702502 A CN 114702502A
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- triazole
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- pyrimidone
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- 150000003852 triazoles Chemical class 0.000 title claims abstract description 111
- VTGOHKSTWXHQJK-UHFFFAOYSA-N pyrimidin-2-ol Chemical compound OC1=NC=CC=N1 VTGOHKSTWXHQJK-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 238000007670 refining Methods 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000003756 stirring Methods 0.000 claims abstract description 58
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 56
- 238000010438 heat treatment Methods 0.000 claims abstract description 40
- 238000001816 cooling Methods 0.000 claims abstract description 32
- 239000000463 material Substances 0.000 claims abstract description 26
- 238000001035 drying Methods 0.000 claims abstract description 22
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000004090 dissolution Methods 0.000 claims abstract description 15
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims abstract description 14
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 claims abstract description 14
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 11
- YCIPQJTZJGUXND-UHFFFAOYSA-N Aglaia odorata Alkaloid Natural products C1=CC(OC)=CC=C1C1(C(C=2C(=O)N3CCCC3=NC=22)C=3C=CC=CC=3)C2(O)C2=C(OC)C=C(OC)C=C2O1 YCIPQJTZJGUXND-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000005070 sampling Methods 0.000 claims abstract description 3
- 238000000967 suction filtration Methods 0.000 claims abstract description 3
- 229920000642 polymer Polymers 0.000 claims description 21
- 239000000047 product Substances 0.000 claims description 19
- -1 triazolopyrimidine ketone Chemical class 0.000 claims description 19
- 239000011259 mixed solution Substances 0.000 claims description 18
- 239000012043 crude product Substances 0.000 claims description 12
- CZPWVGJYEJSRLH-UHFFFAOYSA-N Pyrimidine Chemical compound C1=CN=CN=C1 CZPWVGJYEJSRLH-UHFFFAOYSA-N 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 7
- 239000012452 mother liquor Substances 0.000 abstract description 5
- 238000000746 purification Methods 0.000 abstract description 4
- 238000000926 separation method Methods 0.000 abstract description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical group CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 abstract 2
- 239000012535 impurity Substances 0.000 abstract 1
- 239000000575 pesticide Substances 0.000 description 6
- FIKAKWIAUPDISJ-UHFFFAOYSA-L paraquat dichloride Chemical compound [Cl-].[Cl-].C1=C[N+](C)=CC=C1C1=CC=[N+](C)C=C1 FIKAKWIAUPDISJ-UHFFFAOYSA-L 0.000 description 5
- 231100000419 toxicity Toxicity 0.000 description 3
- 230000001988 toxicity Effects 0.000 description 3
- 239000003814 drug Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- YWBFPKPWMSWWEA-UHFFFAOYSA-O triazolopyrimidine Chemical compound BrC1=CC=CC(C=2N=C3N=CN[N+]3=C(NCC=3C=CN=CC=3)C=2)=C1 YWBFPKPWMSWWEA-UHFFFAOYSA-O 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000002895 emetic Substances 0.000 description 1
- 230000002363 herbicidal effect Effects 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- FFSJPOPLSWBGQY-UHFFFAOYSA-N triazol-4-one Chemical compound O=C1C=NN=N1 FFSJPOPLSWBGQY-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D487/00—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00
- C07D487/02—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00 in which the condensed system contains two hetero rings
- C07D487/04—Ortho-condensed systems
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a method for refining triazolo, which comprises the steps of heating and dissolving crude triazolo and high molecular alcohol until the dissolution is finished, heating the liquid after the dissolution to 80-90 ℃, stirring for 1h, naturally cooling to 60 ℃, cooling to 30 ℃ by using circulating water, carrying out suction filtration on the material after the temperature is reduced to be dry, drying at 80 ℃, carrying out sampling analysis to obtain a triazolo product with the content of 99%, wherein the high molecular alcohol relates to tert-butyl alcohol, n-butyl alcohol, hexanol, octanol and the like, the main impurities in the crude triazolo are triazolo and dipropyl triazolo, the ratio of the crude triazolo to the high molecular alcohol is 1:2-3, the high molecular alcohol adopted during the refining of triazolo has higher solubility to the triazolo, and the slightly soluble to the dipropyl triazolo can well achieve the separation effect, the external standard content of the primarily refined triazole pyrimidinone reaches 99 percent, and the triazole pyrimidinone in the mother liquor can be effectively recovered through secondary purification.
Description
Technical Field
The invention relates to the technical field of pesticide intermediate synthesis, in particular to a method for refining triazole pyrimidinone.
Background
At present, the varieties of pesticides are various, and many pesticides are widely used, but some pesticides have great toxicity to human; for example, paraquat is the second largest biocidal herbicide sold worldwide and has been registered for use in over 100 countries. While the wide use of paraquat is in progress, the toxicity of paraquat is also a particular concern for humans. Because the paraquat has great toxicity to people and no special effect relief medicine, the death rate of oral poisoning can reach more than 90 percent; therefore, in order to improve the safety of related pesticides in the using process, the pesticide parent drug must contain emetic triazolopyrimidine in many countries, so that the harm caused by mistaken eating and toxic events is reduced, and the market prospect of triazolopyrimidine is very good.
Paraquat processing enterprises have high quality requirements on triazolone, and the external standard content is required to be more than 98%. Because the crude product of the triazole pyrimidone contains a large amount of byproduct, namely the dipropyl triazole pyrimidone, which has a similar chemical structure and close physicochemical properties with the product triazole pyrimidone, the content of the product, namely the triazole pyrimidone, can hardly reach more than 98% once by using the conventional refining method, the requirement can be met only by repeated recrystallization, and the triazole pyrimidone taken away from the mother solution is much and is waste, an improved technology is urgently needed to solve the problem in the prior art.
Disclosure of Invention
The invention aims to provide a triazole pyrimidone refining method which adopts high-molecular alcohol with higher solubility to triazole pyrimidone and slightly soluble to dipropyl triazole pyrimidone, can well achieve the separation effect, the external standard content of the once refined triazole pyrimidone reaches 99 percent, and the mother liquor can effectively recover the triazole pyrimidone in the mother liquor through secondary purification, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a method for refining triazole pyrimidinone, which comprises the following steps
Step one, heating and dissolving a crude product of triazole pyrimidone and high molecular alcohol until a clear solution is dissolved;
step two, stirring for 1h, naturally cooling to 60 ℃, and then cooling to 30 ℃ by using circulating water;
step three, filtering the cooled material to be dry, and drying at 80 ℃;
and step four, taking a part of dried samples for analysis to obtain a triazole pyrimidone product with the content of 99%.
Preferably, said method according to step one
S1, purifying the polymer by using tertiary butyl alcohol, n-butyl alcohol, hexanol and octanol, wherein the tertiary butyl alcohol, the n-butyl alcohol, the hexanol and the octanol are mixed according to the ratio of 3: 1: 2: 2, uniformly stirring the proportioned polymer alcohol mixed liquor;
s2, heating the polymer alcohol mixed solution to 80-90 ℃, pouring the crude triazolopyrimidine ketone into the heated polymer alcohol mixed solution, stirring while adding the crude triazolopyrimidine ketone to generate heat, heating the crude triazolopyrimidine ketone and the polymer alcohol to 80-90 ℃ for dissolution until the dissolution is completed, and stirring at a constant speed in one direction all the time during stirring.
Preferably, said method according to step two
S1, heating the liquid after the solution is clear to 80-90 ℃, and stirring at a constant speed for 1 h;
s2, stirring for 1h, naturally cooling to 60 ℃, and then cooling to 30 ℃ by using circulating water.
Preferably, said method according to step three
And S1, carrying out suction filtration on the cooled material until the cooled material is dried, drying the material at 80 ℃, and continuously stirring the material by using a stirrer during drying.
Preferably, the crude triazole pyrimidone product comprises triazole pyrimidine and dipropyl triazole pyrimidone.
Preferably, the ratio of the crude triazole pyrimidone to the high molecular alcohol is 1: 2-3.
Preferably, the dried part of the sample is smashed and ground, the taken sample is mixed with the reaction reagent and then is uniformly stirred, and a sample is taken for analysis to obtain a triazole pyrimidone product with the content of 99%.
Compared with the prior art, the invention has the beneficial effects that:
(1) heating the dissolved and clear liquid to 80-90 ℃, stirring at a constant speed for 1h, naturally cooling to 60 ℃ after stirring for 1h, then cooling to 30 ℃ by using circulating water, and cooling by using circulating water, so that not only is less water used, but also the cooling effect can be ensured;
(3) the polymer alcohol adopted in the refining process of the triazole pyrimidone has higher solubility to the triazole pyrimidone, is slightly soluble to the dipropyl triazole pyrimidone, can well achieve the separation effect, the external standard content of the once refined triazole pyrimidone reaches 99 percent, and the triazole pyrimidone in the mother liquor can be effectively recovered through secondary purification.
Drawings
FIG. 1 is a process diagram of the triazole pyrimidone refining process of the present invention;
FIG. 2 is a chromatogram of the product of example 1 according to the invention;
FIG. 3 is a chromatogram of the product of example 2 of the present invention;
FIG. 4 is a chromatogram of the product of example 3 of the present invention;
FIG. 5 is a chromatogram of a crude product of the present invention;
FIG. 6 is a chromatogram of a product standard of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-6, the present invention provides a technical solution: a method for refining triazole pyrimidinone, which comprises the following steps
Step one, heating and dissolving a crude product of triazole pyrimidone and high molecular alcohol until a clear solution is dissolved;
step two, stirring for 1h, naturally cooling to 60 ℃, and then cooling to 30 ℃ by using circulating water;
step three, filtering the cooled material to be dry, and drying at 80 ℃;
and step four, taking a part of dried samples for analysis to obtain a triazole pyrimidone product with the content of 99%.
Heating and dissolving the crude triazole pyrimidone and high molecular alcohol until the clear solution is dissolved, wherein the high molecular pure comprises tert-butyl alcohol, n-butyl alcohol, hexanol and octanol, and the tert-butyl alcohol, n-butyl alcohol, hexanol and octanol are dissolved according to the ratio of 3: 1: 2: 2, uniformly stirring the proportioned polymer alcohol mixed liquor;
heating the high-molecular alcohol mixed solution to 80-90 ℃, pouring the crude triazole pyrimidone into the heated high-molecular alcohol mixed solution, adding the crude triazole pyrimidone while stirring when the crude triazole pyrimidone is heated, heating the crude triazole pyrimidone and the high-molecular alcohol to 80-90 ℃ for dissolving until the crude triazole pyrimidone is dissolved completely, and stirring at a constant speed in one direction all the time.
Heating the dissolved and clear liquid to 80-90 ℃, stirring at a constant speed for 1h, naturally cooling to 60 ℃ after stirring for 1h, then cooling to 30 ℃ by using circulating water, and cooling by using circulating water, so that not only is less water used, but also the cooling effect can be ensured.
And (2) after the cooled material is filtered to be dry, drying the material at 80 ℃, and continuously stirring by using a stirrer while drying, wherein the crude triazole pyrimidone comprises triazole pyrimidine and dipropyl triazole pyrimidone, and the ratio of the crude triazole pyrimidone to the high molecular alcohol is 1: 2-3.
And (3) smashing and grinding a part of dried samples, mixing the taken samples with a reaction reagent, uniformly stirring, and sampling and analyzing to obtain a triazole pyrimidone product with the content of 99%.
In the case of the example 1, the following examples are given,
when refining the triazole pyrimidone, firstly heating 100g of triazole pyrimidone crude product and 240g of polymer alcohol to 85 ℃ for dissolving until the dissolution is finished;
heating the high-molecular alcohol mixed solution to 80-90 ℃, pouring the crude triazole pyrimidone into the heated high-molecular alcohol mixed solution, adding the crude triazole pyrimidone while stirring when the crude triazole pyrimidone is heated, heating the crude triazole pyrimidone and the high-molecular alcohol to 80-90 ℃ for dissolving until the crude triazole pyrimidone is dissolved completely, and stirring at a constant speed in one direction all the time.
Heating the liquid to 80-90 deg.C, stirring at constant speed for 1h, naturally cooling to 60 deg.C after stirring for 1h, and cooling to 30 deg.C with circulating water.
And (2) after the cooled material is filtered to be dry, drying the material at 80 ℃, and continuously stirring by using a stirrer while drying, wherein the crude triazole pyrimidone comprises triazole pyrimidine and dipropyl triazole pyrimidone, and the ratio of the crude triazole pyrimidone to the high molecular alcohol is 1: 2-3.
Obtaining the weight of a dry product: 65.8 g; the content is as follows: 99.1 percent;
in the case of the example 2, the following examples are given,
when refining the triazole pyrimidone, firstly heating 100g of triazole pyrimidone crude product and 200g of high molecular alcohol to 90 ℃ for dissolution until the dissolution is finished;
heating the high-molecular alcohol mixed solution to 80-90 ℃, pouring the crude triazole pyrimidone into the heated high-molecular alcohol mixed solution, adding the crude triazole pyrimidone while stirring when the crude triazole pyrimidone is heated, heating the crude triazole pyrimidone and the high-molecular alcohol to 80-90 ℃ for dissolving until the crude triazole pyrimidone is dissolved completely, and stirring at a constant speed in one direction all the time.
Heating the liquid to 80-90 deg.C, stirring at constant speed for 1h, naturally cooling to 60 deg.C after stirring for 1h, and cooling to 30 deg.C with circulating water.
And (2) filtering the cooled material to dry, drying the material at 80 ℃, and continuously stirring by using a stirrer while drying, wherein the crude triazole pyrimidinone comprises triazole pyrimidine and dipropyl triazole pyrimidinone, and the ratio of the crude triazole pyrimidinone to the high molecular alcohol is 1: 2-3.
Obtaining the weight of a dry product: 62.6 g; the content is as follows: 99.2 percent;
in the case of the example 3, the following examples are given,
when refining the triazole pyrimidone, firstly heating 100g of triazole pyrimidone crude product and 160g of high molecular alcohol to dissolve at 95 ℃ until the dissolution is finished;
heating the polymer alcohol mixed solution to 80-90 ℃, pouring the crude triazole pyrimidone into the heated polymer alcohol mixed solution, stirring while adding the crude triazole pyrimidone to generate heat, heating the crude triazole pyrimidone and the polymer alcohol to 80-90 ℃, dissolving until the dissolution is finished, and stirring at a constant speed in one direction all the time.
Heating the liquid to 80-90 deg.C, stirring at constant speed for 1h, naturally cooling to 60 deg.C after stirring for 1h, and cooling to 30 deg.C with circulating water.
And (2) after the cooled material is filtered to be dry, drying the material at 80 ℃, and continuously stirring by using a stirrer while drying, wherein the crude triazole pyrimidone comprises triazole pyrimidine and dipropyl triazole pyrimidone, and the ratio of the crude triazole pyrimidone to the high molecular alcohol is 1: 2-3.
Obtaining the weight of a dry product: 60.6 g; the content is as follows: 99.3 percent;
in the case of the example 4, it is preferred,
when refining the triazole pyrimidone, firstly heating 100g of triazole pyrimidone crude product and 120g of polymer alcohol to dissolve at 90 ℃ until the dissolution is finished;
heating the high-molecular alcohol mixed solution to 80-90 ℃, pouring the crude triazole pyrimidone into the heated high-molecular alcohol mixed solution, adding the crude triazole pyrimidone while stirring when the crude triazole pyrimidone is heated, heating the crude triazole pyrimidone and the high-molecular alcohol to 80-90 ℃ for dissolving until the crude triazole pyrimidone is dissolved completely, and stirring at a constant speed in one direction all the time.
Heating the dissolved and clear liquid to 80-90 ℃, stirring at constant speed for 1h, naturally cooling to 60 ℃ after stirring for 1h, and then cooling to 30 ℃ by using circulating water.
And (2) after the cooled material is filtered to be dry, drying the material at 80 ℃, and continuously stirring by using a stirrer while drying, wherein the crude triazole pyrimidone comprises triazole pyrimidine and dipropyl triazole pyrimidone, and the ratio of the crude triazole pyrimidone to the high molecular alcohol is 1: 2-3.
Obtaining the weight of a dry product: 56.6 g; the content is as follows: 99.4 percent;
in the case of the example 5, the following examples were conducted,
when refining the triazole pyrimidone, firstly heating 100g of triazole pyrimidone crude product and 90g of high molecular alcohol to dissolve at 95 ℃ until the dissolution is finished;
heating the high-molecular alcohol mixed solution to 80-90 ℃, pouring the crude triazole pyrimidone into the heated high-molecular alcohol mixed solution, adding the crude triazole pyrimidone while stirring when the crude triazole pyrimidone is heated, heating the crude triazole pyrimidone and the high-molecular alcohol to 80-90 ℃ for dissolving until the crude triazole pyrimidone is dissolved completely, and stirring at a constant speed in one direction all the time.
Heating the liquid to 80-90 deg.C, stirring at constant speed for 1h, naturally cooling to 60 deg.C after stirring for 1h, and cooling to 30 deg.C with circulating water.
And (2) after the cooled material is filtered to be dry, drying the material at 80 ℃, and continuously stirring by using a stirrer while drying, wherein the crude triazole pyrimidone comprises triazole pyrimidine and dipropyl triazole pyrimidone, and the ratio of the crude triazole pyrimidone to the high molecular alcohol is 1: 2-3.
Obtaining the weight of a dry product: 52.6 g; the content is as follows: 99.5 percent;
in the case of the example 6, it is shown,
when refining the triazole pyrimidone, firstly heating 100g of triazole pyrimidone crude product and 60g of high molecular alcohol to dissolve at 95 ℃ until the dissolution is finished;
heating the polymer alcohol mixed solution to 80-90 ℃, pouring the crude triazole pyrimidone into the heated polymer alcohol mixed solution, stirring while adding the crude triazole pyrimidone to generate heat, heating the crude triazole pyrimidone and the polymer alcohol to 80-90 ℃, dissolving until the dissolution is finished, and stirring at a constant speed in one direction all the time.
Heating the liquid to 80-90 deg.C, stirring at constant speed for 1h, naturally cooling to 60 deg.C after stirring for 1h, and cooling to 30 deg.C with circulating water.
And (2) after the cooled material is filtered to be dry, drying the material at 80 ℃, and continuously stirring by using a stirrer while drying, wherein the crude triazole pyrimidone comprises triazole pyrimidine and dipropyl triazole pyrimidone, and the ratio of the crude triazole pyrimidone to the high molecular alcohol is 1: 2-3.
Obtaining the weight of a dry product: 50.8 g; the content is as follows: 99.6 percent;
the polymer alcohol adopted in the refining process of the triazole pyrimidone has higher solubility to the triazole pyrimidone, is slightly soluble to the dipropyl triazole pyrimidone, can well achieve the separation effect, the external standard content of the once refined triazole pyrimidone reaches 99 percent, and the triazole pyrimidone in the mother liquor can be effectively recovered through secondary purification.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A method for refining triazole pyrimidone is characterized by comprising the following steps: the above-mentioned
Step one, heating and dissolving a crude product of triazole pyrimidone and high molecular alcohol until a clear solution is dissolved;
step two, stirring for 1h, naturally cooling to 60 ℃, and then cooling to 30 ℃ by using circulating water;
step three, filtering the cooled material to be dry, and drying at 80 ℃;
and step four, taking a part of dried samples for analysis to obtain a triazole pyrimidone product with the content of 99%.
2. The method for refining triazole pyrimidone according to claim 1, which is characterized in that: the method comprises the following steps of
S1, purifying the polymer by using tertiary butyl alcohol, n-butyl alcohol, hexanol and octanol, wherein the tertiary butyl alcohol, the n-butyl alcohol, the hexanol and the octanol are mixed according to the ratio of 3: 1: 2: 2, uniformly stirring the proportioned polymer alcohol mixed liquor;
s2, heating the polymer alcohol mixed solution to 80-90 ℃, pouring the crude triazolopyrimidine ketone into the heated polymer alcohol mixed solution, stirring while adding the crude triazolopyrimidine ketone to generate heat, heating the crude triazolopyrimidine ketone and the polymer alcohol to 80-90 ℃ for dissolution until the dissolution is completed, and stirring at a constant speed in one direction all the time during stirring.
3. The method for refining triazole pyrimidone according to claim 1, which is characterized in that: the step two
S1, heating the liquid after the solution is clear to 80-90 ℃, and stirring at a constant speed for 1 h;
s2, stirring for 1h, naturally cooling to 60 ℃, and then cooling to 30 ℃ by using circulating water.
4. The method for refining triazole pyrimidone according to claim 1, which is characterized in that: the step three is described
And S1, carrying out suction filtration on the cooled material until the cooled material is dried, drying the material at 80 ℃, and continuously stirring the material by using a stirrer during drying.
5. The method for refining triazole pyrimidone according to claim 1, which is characterized in that: the crude product of triazole pyrimidinone comprises triazole pyrimidine and dipropyl triazole pyrimidinone.
6. The method for refining triazole pyrimidone according to claim 1, which is characterized in that: the ratio of the crude triazole pyrimidone to the high molecular alcohol is 1: 2-3.
7. The method for refining triazole pyrimidone according to claim 1, which is characterized in that: and (3) smashing and grinding a part of dried samples, mixing the taken samples with a reaction reagent, uniformly stirring, and sampling and analyzing to obtain a triazole pyrimidone product with the content of 99%.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109503588A (en) * | 2018-11-15 | 2019-03-22 | 江苏诺恩作物科学股份有限公司 | A kind of triazole pyrimidone preparation method |
| CN109575031A (en) * | 2018-11-15 | 2019-04-05 | 江苏诺恩作物科学股份有限公司 | A kind of preparation method of emetic |
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- 2022-05-19 CN CN202210545817.1A patent/CN114702502A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109503588A (en) * | 2018-11-15 | 2019-03-22 | 江苏诺恩作物科学股份有限公司 | A kind of triazole pyrimidone preparation method |
| CN109575031A (en) * | 2018-11-15 | 2019-04-05 | 江苏诺恩作物科学股份有限公司 | A kind of preparation method of emetic |
Non-Patent Citations (1)
| Title |
|---|
| 叶彦春，郭燕文，黄学斌主编: "《有机化学实验 第2版》", 28 February 2014 * |
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Application publication date: 20220705 |