CN108752195A - A kind of new preparation process of 2,4- dihydroxybenzoyls chlorine - Google Patents
A kind of new preparation process of 2,4- dihydroxybenzoyls chlorine Download PDFInfo
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- CN108752195A CN108752195A CN201810788021.2A CN201810788021A CN108752195A CN 108752195 A CN108752195 A CN 108752195A CN 201810788021 A CN201810788021 A CN 201810788021A CN 108752195 A CN108752195 A CN 108752195A
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- CN
- China
- Prior art keywords
- added
- chlorine
- new preparation
- dihydroxybenzoyls
- preparation process
- Prior art date
- 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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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/58—Preparation of carboxylic acid halides
- C07C51/60—Preparation of carboxylic acid halides by conversion of carboxylic acids or their anhydrides or esters, lactones, salts into halides with the same carboxylic acid part
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The title of the present invention is a kind of new preparation process of 2,4- dihydroxy benzenes acyl chlorides.Affiliated technical field is medical science.The technical problems to be solved by the invention are to be related to a kind of new preparation process of more advanced 2,4- dihydroxybenzoyls chlorine.The main points of the technical solution of the technical problems to be solved by the invention are a kind of new preparation methods of the compound.
Description
Technical field
The present invention relates to pharmaceutical technology fields, specifically, the present invention relates to the new of one kind 2,4- dihydroxybenzoyl chlorine
Preparation method.
Background technology
2,4- dihydroxybenzoyl chlorine are a kind of intermediate feeds of important synthesis medical product.
The preparation method yield of existing 2,4- dihydroxybenzoyls chlorine is not high, and synthesis technology is complicated, and yield is unstable, needs
A kind of new preparation method is invented, to overcome the shortcomings of prior art, to achieve the purpose that energy-saving and environmental protection, green.
Invention content
The present invention uses a kind of new technology, not high for the preparation method yield of existing 2,4- dihydroxybenzoyls chlorine,
Synthesis technology is complicated, and yield is unstable, and the disadvantage that the purchase cost of required raw material is high has invented one by long-term research and development
The new preparation method of kind has established good technical foundation to overcome the shortcomings of prior art for later industrial production.
The technical scheme is that：
1541 milligrams of 2,4- dihydroxy-benzoic acids are added in the reactor, 30 milliliters of tetrahydrofuran, in stirring, room is added
0.5 milliliter of n,N-Dimethylformamide is added in middle benefit gas, is then stirred at room temperature 0.5 hour, 3 grams of thionyl chloride is added dropwise, then
Continue to be stirred to react at room temperature 8 hours.After completion of the reaction, post-treated and purification process obtains compound 2,4- dihydroxy
Chlorobenzoyl chloride, yield 89.8%.
Specific implementation mode
Embodiment 1：The preparation of 2,4- dihydroxybenzoyl chlorine：
1541 milligrams of 2,4- dihydroxy-benzoic acids are added in the reactor, 30 milliliters of tetrahydrofuran, in stirring, room is added
0.5 milliliter of n,N-Dimethylformamide is added in middle benefit gas, is then stirred at room temperature 0.5 hour, 3 grams of thionyl chloride is added dropwise, then
Continue to be stirred to react at room temperature 8 hours.After completion of the reaction, post-treated and purification process obtains compound 2,4- dihydroxy
Chlorobenzoyl chloride, yield 89.8%.
Embodiment 2：The preparation of 2,4- dihydroxybenzoyl chlorine：
1541 milligrams of 2,4- dihydroxy-benzoic acids are added in the reactor, 30 milliliters of tetrahydrofuran, in stirring, room is added
0.5 milliliter of n,N-Dimethylformamide is added in middle benefit gas, is then stirred at room temperature 0.5 hour, 3 grams of thionyl chloride is added dropwise, then
Continue to be stirred to react at room temperature 8 hours.After completion of the reaction, post-treated and purification process obtains compound 2,4- dihydroxy
Chlorobenzoyl chloride, yield 90.4%.
The present invention can be summarized with others without prejudice to the concrete form of the spirit or essential characteristics of the present invention.Therefore, nothing
By from the point of view of which point, the embodiment above of the invention can only all be considered the description of the invention and cannot limit this hair
It is bright.
Claims (2)
1. one kind 2, the new preparation process of 4- dihydroxy formyl chlorides, it is characterized in that：
1541 milligrams of 2,4- dihydroxy-benzoic acids are added in the reactor, 30 milliliters of tetrahydrofuran is added, in stirring, add in room temperature
Enter 0.5 milliliter of n,N-Dimethylformamide, be then stirred at room temperature 0.5 hour, 3 grams of thionyl chloride is added dropwise, then continues
It is stirred to react in room temperature 8 hours.After completion of the reaction, post-treated and purification process obtains compound 2,4- dihydroxybenzoyls
Chlorine, yield 89.8%.
2. according to the method described in claim 1, it is characterized in that:
It needs that compound N, dinethylformamide is added in reaction solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810788021.2A CN108752195A (en) | 2018-07-18 | 2018-07-18 | A kind of new preparation process of 2,4- dihydroxybenzoyls chlorine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810788021.2A CN108752195A (en) | 2018-07-18 | 2018-07-18 | A kind of new preparation process of 2,4- dihydroxybenzoyls chlorine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108752195A true CN108752195A (en) | 2018-11-06 |
Family
ID=63970463
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810788021.2A Pending CN108752195A (en) | 2018-07-18 | 2018-07-18 | A kind of new preparation process of 2,4- dihydroxybenzoyls chlorine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108752195A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105968244A (en) * | 2016-06-28 | 2016-09-28 | 河南工业大学 | Phenolic hydroxyl benzoate based macromolecular antibacterial material preparation method |
| CN106866419A (en) * | 2017-04-14 | 2017-06-20 | 石河子大学 | One terpenoid ester compounds and its production and use |
-
2018
- 2018-07-18 CN CN201810788021.2A patent/CN108752195A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105968244A (en) * | 2016-06-28 | 2016-09-28 | 河南工业大学 | Phenolic hydroxyl benzoate based macromolecular antibacterial material preparation method |
| CN106866419A (en) * | 2017-04-14 | 2017-06-20 | 石河子大学 | One terpenoid ester compounds and its production and use |
Non-Patent Citations (2)
| Title |
|---|
| L.G.DERKACH等: "Esterification of 2,4-Dihydroxybenzoic Acid", 《RUSSIAN JOURNAL OF ORGANIC CHEMISTRY》 * |
| NEVENA IVANOVIC等: "Potent 1,2,4-Triazole-3-thione Radical Scavengers Derived from Phenolic Acids: Synthesis, Electrochemistry, and Theoretical Study", 《CHEMISTRYSELECT》 * |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20181106 |
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| WD01 | Invention patent application deemed withdrawn after publication |