CN104370826A - Preparation method of 5-methoxyl-4,6-dichloro pyrimidine - Google Patents
Preparation method of 5-methoxyl-4,6-dichloro pyrimidine Download PDFInfo
- Publication number
- CN104370826A CN104370826A CN201410760577.2A CN201410760577A CN104370826A CN 104370826 A CN104370826 A CN 104370826A CN 201410760577 A CN201410760577 A CN 201410760577A CN 104370826 A CN104370826 A CN 104370826A
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- China
- Prior art keywords
- trieline
- methoxyl
- mass parts
- methoxyl group
- dichloro pyrimidine
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D239/00—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings
- C07D239/02—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings
- C07D239/24—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members
- C07D239/28—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, directly attached to ring carbon atoms
- C07D239/32—One oxygen, sulfur or nitrogen atom
- C07D239/34—One oxygen atom
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention discloses a preparation method of 5-methoxyl-4,6-dichloro pyrimidine. The method includes the steps of firstly, adding 31 parts of 5-methoxyl-4,6-dihydroxy pyrimidine disodium and 42 parts of phosphorus oxychloride into a reaction kettle, keeping the temperature at 65 DEG C for 1.5 hours, and reducing pressure to recycle phosphorus oxychloride until the material is dried; secondly, cooling to 35 DEG C, adding trichloro ethylene, placing into a hydrolysis pot, adding 650 parts of water, and stirring at 65 DEG C; thirdly, removing the trichloro ethylene layer, adding the trichloro ethylene again, repeatedly extracting for 9 times, and placing the trichloro ethylene layer into a distillatory kettle to recycle the trichloro ethylene so as to obtain coarse chloride; fourthly, adding the coarse chloride into a refining kettle, adding methanol three times as much as the coarse chloride, heating to achieve full dissolution, cooling to 45 DEG C, and discharging and drying to obtain 19 parts of 5-methoxyl-4,6-dichloro pyrimidine. The method is high in 5-methoxyl-4,6-dichloro pyrimidine yield.
Description
Technical field
The present invention relates to the preparation method of 5-methoxyl group-4,6-dichloro pyrimidine.
Background technology
The preparation method of existing 5-methoxyl group-4,6-dichloro pyrimidine, yield is low.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of 5-methoxyl group-4,6-dichloro pyrimidine, its 5-methoxyl group-4,6-dichloro pyrimidine yield prepared is high.
For achieving the above object, technical scheme of the present invention designs a kind of preparation method of 5-methoxyl group-4,6-dichloro pyrimidine, comprises the steps:
1) drop into 31 mass parts 5-methoxyl group-4,6-dihydroxy pyrimidine disodiums and 42 mass parts Phosphorus Oxychlorides in a kettle., 65 DEG C are incubated 1.5 hours, and reclaim under reduced pressure Phosphorus Oxychloride is dry to material;
2) be cooled to 35 DEG C, add trieline, put in hydrolyzer, then put into 650 mass parts water, 65 DEG C of stirrings;
3) divide and remove trieline layer, then add trieline, extracting 9 times repeatedly, trieline layer is put into still pot and is reclaimed trieline, obtains thick muriate;
4) dropped in refining kettle thick muriate, add the methyl alcohol of 3 times amount, be cooled to 45 DEG C after heating is entirely molten, discharging is dried, and obtains 19 mass parts 5-methoxyl group-4,6-dichloro pyrimidines.
Advantage of the present invention and beneficial effect are: the preparation method providing a kind of 5-methoxyl group-4,6-dichloro pyrimidine, and its 5-methoxyl group-4,6-dichloro pyrimidine yield prepared is high.
Embodiment
Below in conjunction with embodiment, the specific embodiment of the present invention is further described.Following examples only for technical scheme of the present invention is clearly described, and can not limit the scope of the invention with this.
The technical scheme that the present invention specifically implements is:
A kind of preparation method of 5-methoxyl group-4,6-dichloro pyrimidine, comprises the steps:
1) drop into 31 mass parts 5-methoxyl group-4,6-dihydroxy pyrimidine disodiums and 42 mass parts Phosphorus Oxychlorides in a kettle., 65 DEG C are incubated 1.5 hours, and reclaim under reduced pressure Phosphorus Oxychloride is dry to material;
2) be cooled to 35 DEG C, add trieline, put in hydrolyzer, then put into 650 mass parts water, 65 DEG C of stirrings;
3) divide and remove trieline layer, then add trieline, extracting 9 times repeatedly, trieline layer is put into still pot and is reclaimed trieline, obtains thick muriate;
4) dropped in refining kettle thick muriate, add the methyl alcohol of 3 times amount, be cooled to 45 DEG C after heating is entirely molten, discharging is dried, and obtains 19 mass parts 5-methoxyl group-4,6-dichloro pyrimidines.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (1)
- The preparation method of 1.5-methoxyl group-4,6-dichloro pyrimidine, is characterized in that, comprise the steps:1) drop into 31 mass parts 5-methoxyl group-4,6-dihydroxy pyrimidine disodiums and 42 mass parts Phosphorus Oxychlorides in a kettle., 65 DEG C are incubated 1.5 hours, and reclaim under reduced pressure Phosphorus Oxychloride is dry to material;2) be cooled to 35 DEG C, add trieline, put in hydrolyzer, then put into 650 mass parts water, 65 DEG C of stirrings;3) divide and remove trieline layer, then add trieline, extracting 9 times repeatedly, trieline layer is put into still pot and is reclaimed trieline, obtains thick muriate;4) dropped in refining kettle thick muriate, add the methyl alcohol of 3 times amount, be cooled to 45 DEG C after heating is entirely molten, discharging is dried, and obtains 19 mass parts 5-methoxyl group-4,6-dichloro pyrimidines.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410760577.2A CN104370826B (en) | 2014-12-13 | 2014-12-13 | Preparation method of 5-methoxyl-4,6-dichloro pyrimidine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410760577.2A CN104370826B (en) | 2014-12-13 | 2014-12-13 | Preparation method of 5-methoxyl-4,6-dichloro pyrimidine |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104370826A true CN104370826A (en) | 2015-02-25 |
| CN104370826B CN104370826B (en) | 2017-01-11 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410760577.2A Active CN104370826B (en) | 2014-12-13 | 2014-12-13 | Preparation method of 5-methoxyl-4,6-dichloro pyrimidine |
Country Status (1)
| Country | Link |
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| CN (1) | CN104370826B (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864701A (en) * | 2014-03-10 | 2014-06-18 | 常熟市金申医化制品有限责任公司 | Preparation method of 4-sulfanilamide-5-methoxyl-6-chloropyrimidine |
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2014
- 2014-12-13 CN CN201410760577.2A patent/CN104370826B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864701A (en) * | 2014-03-10 | 2014-06-18 | 常熟市金申医化制品有限责任公司 | Preparation method of 4-sulfanilamide-5-methoxyl-6-chloropyrimidine |
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| Publication number | Publication date |
|---|---|
| CN104370826B (en) | 2017-01-11 |
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Address after: 215500 Xinyu village, Shanghu Town, Changshu City, Suzhou City, Jiangsu Province Patentee after: Jiangsu Jinshen Pharmaceutical Technology Co., Ltd Address before: 215500 No.8, Xinyu village, Shanghu Town, Changshu City, Suzhou City, Jiangsu Province Patentee before: CHANGSHU JINSHEN MEDICAL CHEMISTRY PRODUCTS Co.,Ltd. |