CN102827085A - Preparation method for 2,4,5-trichloropyrimidine compound - Google Patents
Preparation method for 2,4,5-trichloropyrimidine compound Download PDFInfo
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- CN102827085A CN102827085A CN2012103452868A CN201210345286A CN102827085A CN 102827085 A CN102827085 A CN 102827085A CN 2012103452868 A CN2012103452868 A CN 2012103452868A CN 201210345286 A CN201210345286 A CN 201210345286A CN 102827085 A CN102827085 A CN 102827085A
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- Prior art keywords
- trichloropyrimidine
- preparation
- compound
- chlorouracil
- few
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Abstract
The invention discloses a preparation method for 2,4,5-trichloropyrimidine compound. The method comprises the following steps of adding 5-chlorouracil and thionyl chloride in dichloroethane solvent, performing heat insulation reflux reaction, after the reflux is finished, adding water in the mixture, separating the water layer, and performing distillation to distil the dichloroethane from the mixture, and thus obtaining 2,4,5-trichloropyrimidine. According to the method provided by the invention, new chlorinating agent is adopted to replace the original technology, the amount of the chlorinating agent is few, the process is easy in control, the sewage discharge is few, no phosphide pollution exists; the production cost is greatly reduced; the product quality is stable; and the product has a very favorable position in future domestic and international competition.
Description
Technical field
The invention belongs to compound field, particularly relate to 2,4, the preparation method of 5-trichloropyrimidine compound with pyrimidine structure.
Background technology
2,4, the 5-trichloropyrimidine is the synthesis material of a kind of new reactive dyes intermediate feed and the new chemical medicine of Azelaic Acid; Continuous increase along with new reactive dyes and Azelaic Acid new drug sales volume; Its synthetic required raw material 2,4, the demand of 5-trichloropyrimidine is also in continuous growth; Therefore to its synthetic research, develop the novel environment-friendly process that is fit to industrialized production and seem particularly urgent.This product domestic corporation adopts traditional technology basically at present, and working condition is harsh, and environmental pollution is more serious.
Summary of the invention
The object of the present invention is to provide a kind of technology controlling and process easy, sewage discharge is few, 2,4 of no phosphide pollution, the preparation method of 5-trichloropyrimidine compound.
Technical solution of the present invention is:
A kind of 2,4, the preparation method of 5-trichloropyrimidine compound is characterized in that: comprise the steps:
In the solvent ethylene dichloride, drop into 5-chlorouracil and sulfur oxychloride, the insulation back flow reaction, backflow finishes, and adds entry, and branch vibration layer distills then, boils off ethylene dichloride, gets 2,4, the 5-trichloropyrimidine.
The mol ratio of 5-chlorouracil and sulfur oxychloride is 1:1-30; The insulation reflux time is 1-60 hour.
Chemosynthesis reaction equation of the present invention is following:
The present invention adopts new chlorizating agent to replace original technology, and the chlorizating agent consumption is few, and technology controlling and process is easy; Sewage discharge is few, and no phosphide pollutes, and production cost reduces greatly; Constant product quality, this product all will be in very favorable status in the domestic and even international competition in future.
Reaction times short reaction process of the present invention is carried out under normal pressure, and is easy and simple to handle; Product yield and purity are all higher, and yield is more than 80%, and purity reaches more than 99%.
Below in conjunction with embodiment the present invention is described further.
Embodiment
A kind of 2,4, the preparation method of 5-trichloropyrimidine compound comprises the steps: in the solvent ethylene dichloride, drops into 5-chlorouracil and sulfur oxychloride; The insulation back flow reaction, backflow finishes, and adds entry, and branch vibration layer distills then; Boil off ethylene dichloride, get 2,4, the 5-trichloropyrimidine.The mol ratio of 5-chlorouracil and sulfur oxychloride is 1: 1-30 (example 1: 1,1: 15,1: 30); The insulation reflux time is 1-60 hour (routine 1h, 30h, 60h).Yield is more than 80%, and purity reaches more than 99%.
Claims (2)
1. one kind 2,4, the preparation method of 5-trichloropyrimidine compound is characterized in that: comprise the steps:
In the solvent ethylene dichloride, drop into 5-chlorouracil and sulfur oxychloride, the insulation back flow reaction, backflow finishes, and adds entry, and branch vibration layer distills then, boils off ethylene dichloride, gets 2,4, the 5-trichloropyrimidine.
2. according to claim 12,4, the preparation method of 5-trichloropyrimidine compound is characterized in that: the mol ratio of 5-chlorouracil and sulfur oxychloride is 1:1-30; The insulation reflux time is 1-60 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103452868A CN102827085A (en) | 2012-09-17 | 2012-09-17 | Preparation method for 2,4,5-trichloropyrimidine compound |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103452868A CN102827085A (en) | 2012-09-17 | 2012-09-17 | Preparation method for 2,4,5-trichloropyrimidine compound |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102827085A true CN102827085A (en) | 2012-12-19 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012103452868A Pending CN102827085A (en) | 2012-09-17 | 2012-09-17 | Preparation method for 2,4,5-trichloropyrimidine compound |
Country Status (1)
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| CN (1) | CN102827085A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113912550A (en) * | 2021-11-11 | 2022-01-11 | 浙江先锋科技股份有限公司 | Method for preparing 2,4, 5-trichloropyrimidine |
| CN115677595A (en) * | 2022-10-26 | 2023-02-03 | 江苏睿实生物科技有限公司 | Preparation method of 2,4, 5-trichloropyrimidine |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6046206A (en) * | 1995-06-07 | 2000-04-04 | Cell Pathways, Inc. | Method of treating a patient having a precancerous lesions with amide quinazoline derivatives |
| WO2004016597A2 (en) * | 2002-08-14 | 2004-02-26 | Vertex Pharmaceuticals Incorporated | Protein kinase inhibitors and uses thereof |
| US20060025433A1 (en) * | 2004-07-08 | 2006-02-02 | Boehringer Ingelheim Pharmaceuticals, Inc. | Pyrimidine derivatives useful as inhibitors of PKC-theta |
| WO2007120339A1 (en) * | 2005-12-19 | 2007-10-25 | Genentech, Inc. | Pyrimidine kinase inhibitors |
| CN101563327A (en) * | 2006-12-19 | 2009-10-21 | 健泰科生物技术公司 | Pyrimidine kinase inhibitors |
| WO2010118367A2 (en) * | 2009-04-10 | 2010-10-14 | Progenics Pharmaceuticals, Inc. | Antiviral pyrimidines |
-
2012
- 2012-09-17 CN CN2012103452868A patent/CN102827085A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6046206A (en) * | 1995-06-07 | 2000-04-04 | Cell Pathways, Inc. | Method of treating a patient having a precancerous lesions with amide quinazoline derivatives |
| WO2004016597A2 (en) * | 2002-08-14 | 2004-02-26 | Vertex Pharmaceuticals Incorporated | Protein kinase inhibitors and uses thereof |
| US20060025433A1 (en) * | 2004-07-08 | 2006-02-02 | Boehringer Ingelheim Pharmaceuticals, Inc. | Pyrimidine derivatives useful as inhibitors of PKC-theta |
| WO2007120339A1 (en) * | 2005-12-19 | 2007-10-25 | Genentech, Inc. | Pyrimidine kinase inhibitors |
| CN101563327A (en) * | 2006-12-19 | 2009-10-21 | 健泰科生物技术公司 | Pyrimidine kinase inhibitors |
| WO2010118367A2 (en) * | 2009-04-10 | 2010-10-14 | Progenics Pharmaceuticals, Inc. | Antiviral pyrimidines |
Non-Patent Citations (2)
| Title |
|---|
| HAN WANG等: "Large-Scale Solvent-Free Chlorination of Hydroxy-Pyrimidines,-Pyridines, -Pyrazines and -Amides Using Equimolar POCl3", 《MOLECULES》 * |
| ZHIYUAN ZHANG等: "Design and Synthesis of Pyrimidinone and Pyrimidinedione Inhibitors of Dipeptidyl Peptidase IV", 《JOURNAL OF MEDICINAL CHEMISTRY》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113912550A (en) * | 2021-11-11 | 2022-01-11 | 浙江先锋科技股份有限公司 | Method for preparing 2,4, 5-trichloropyrimidine |
| CN115677595A (en) * | 2022-10-26 | 2023-02-03 | 江苏睿实生物科技有限公司 | Preparation method of 2,4, 5-trichloropyrimidine |
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Application publication date: 20121219 |