CN108689835A - A kind of new preparation process of 3- hydroxybenzoyl chlorides - Google Patents
A kind of new preparation process of 3- hydroxybenzoyl chlorides Download PDFInfo
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- CN108689835A CN108689835A CN201810753652.0A CN201810753652A CN108689835A CN 108689835 A CN108689835 A CN 108689835A CN 201810753652 A CN201810753652 A CN 201810753652A CN 108689835 A CN108689835 A CN 108689835A
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- hydroxybenzoyl
- chlorides
- new preparation
- preparation process
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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 3- hydroxybenzoyl 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 3- hydroxybenzoyl chlorides.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 a kind of the freshly prepared of 3- hydroxybenzoyl chlorides
Method.
Background technology
3- hydroxybenzoyl chlorides are a kind of intermediate feeds of important synthesis medical product.
The preparation method yield of existing 3- hydroxybenzoyl chlorides is not high, and synthesis technology is complicated, and yield is unstable, needs to send out
Bright a kind of new preparation method, 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 3- hydroxybenzoyl chlorides, synthesis
Complex process, yield is unstable, and the disadvantage that the purchase cost of required raw material is high has been invented a kind of new by long-term research and development
Preparation method established good technical foundation to overcome the shortcomings of prior art for later industrial production.
The technical scheme is that:
1381 milligrams of 3- hydroxybenzoic acids are added in the reactor, 50 milliliters of toluene is added, in stirring, 3 are added in room temperature
The n,N-Dimethylformamide of milliliter, is then stirred at room temperature 20 minutes, then the temperature of reaction solution is heated to 60 DEG C in oil bath,
3 grams of thionyl chloride is added dropwise, then continues to be stirred to react in 60 DEG C 4 hours.After completion of the reaction, it is post-treated with purified
Journey obtains compound 3- hydroxybenzoyl chlorides, yield 73.6%.
Specific implementation mode
Embodiment 1:The preparation of 3- hydroxybenzoyl chlorides:
1381 milligrams of 3- hydroxybenzoic acids are added in the reactor, 50 milliliters of toluene is added, in stirring, 3 are added in room temperature
The n,N-Dimethylformamide of milliliter, is then stirred at room temperature 20 minutes, then the temperature of reaction solution is heated to 60 DEG C in oil bath,
3 grams of thionyl chloride is added dropwise, then continues to be stirred to react in 60 DEG C 4 hours.After completion of the reaction, it is post-treated with purified
Journey obtains compound 3- hydroxybenzoyl chlorides, yield 73.6%.
Embodiment 2:The preparation of 3- hydroxybenzoyl chlorides:
1381 milligrams of 3- hydroxybenzoic acids are added in the reactor, 50 milliliters of toluene is added, in stirring, 3 are added in room temperature
The n,N-Dimethylformamide of milliliter, is then stirred at room temperature 20 minutes, then the temperature of reaction solution is heated to 60 DEG C in oil bath,
3 grams of thionyl chloride is added dropwise, then continues to be stirred to react in 60 DEG C 4 hours.After completion of the reaction, it is post-treated with purified
Journey obtains compound 3- hydroxybenzoyl chlorides, yield 76.3%.
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. a kind of new preparation process of 3- hydroxybenzoyl chlorides, it is characterized in that:
1381 milligrams of 3- hydroxybenzoic acids are added in the reactor, 50 milliliters of toluene is added, in stirring, 3 milliliters are added in room temperature
N,N-Dimethylformamide, be then stirred at room temperature 20 minutes, then the temperature of reaction solution is heated to 60 DEG C in oil bath, be added dropwise
Then 3 grams of thionyl chloride continues to be stirred to react in 60 DEG C 4 hours.After completion of the reaction, post-treated and purification process, obtains
To compound 3- hydroxybenzoyl chlorides, yield 73.6%.
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 |
|---|---|---|---|
| CN201810753652.0A CN108689835A (en) | 2018-07-10 | 2018-07-10 | A kind of new preparation process of 3- hydroxybenzoyl chlorides |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810753652.0A CN108689835A (en) | 2018-07-10 | 2018-07-10 | A kind of new preparation process of 3- hydroxybenzoyl chlorides |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108689835A true CN108689835A (en) | 2018-10-23 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810753652.0A Pending CN108689835A (en) | 2018-07-10 | 2018-07-10 | A kind of new preparation process of 3- hydroxybenzoyl chlorides |
Country Status (1)
| Country | Link |
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| CN (1) | CN108689835A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101376627A (en) * | 2008-09-26 | 2009-03-04 | 上海应用技术学院 | Preparation of 4-hydroxybenzoyl chloride |
| CN102531946A (en) * | 2012-01-05 | 2012-07-04 | 山东大学 | 3-methoxybenzamide (MBA) derivant as well as preparation method and application thereof |
| CN107619369A (en) * | 2016-07-13 | 2018-01-23 | 北京旭阳科技有限公司 | A kind of method for synthesizing m-hydroxybenzaldehyde |
-
2018
- 2018-07-10 CN CN201810753652.0A patent/CN108689835A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101376627A (en) * | 2008-09-26 | 2009-03-04 | 上海应用技术学院 | Preparation of 4-hydroxybenzoyl chloride |
| CN102531946A (en) * | 2012-01-05 | 2012-07-04 | 山东大学 | 3-methoxybenzamide (MBA) derivant as well as preparation method and application thereof |
| CN107619369A (en) * | 2016-07-13 | 2018-01-23 | 北京旭阳科技有限公司 | A kind of method for synthesizing m-hydroxybenzaldehyde |
Non-Patent Citations (1)
| Title |
|---|
| 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: 20181023 |
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| WD01 | Invention patent application deemed withdrawn after publication |