CN108794328A - The preparation method of 3,4- dimethoxy-benzoyl chlorides - Google Patents
The preparation method of 3,4- dimethoxy-benzoyl chlorides Download PDFInfo
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- CN108794328A CN108794328A CN201810875471.5A CN201810875471A CN108794328A CN 108794328 A CN108794328 A CN 108794328A CN 201810875471 A CN201810875471 A CN 201810875471A CN 108794328 A CN108794328 A CN 108794328A
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- added
- dimethoxy
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- benzoyl chlorides
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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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- 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 the preparation method of 3,4- dimethoxy-benzoyl chlorides.Affiliated technical field is medical science.The technical problems to be solved by the invention are to be related to a kind of preparation method of more advanced 3,4- dimethoxy-benzoyl 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 3, the preparation of 4- dimethoxy-benzoyl chlorides
Method.
Background technology
3,4- dimethoxy-benzoyl chlorides are a kind of intermediate feeds of important synthesis medical product.
The preparation method yield of existing 3,4- dimethoxy-benzoyl chlorides is not high, and synthesis technology is complicated, and yield is unstable,
It needs to invent 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 use a kind of new technology, for existing 3,4- dimethoxy-benzoyl chlorides preparation method yield not
Height, synthesis technology is complicated, and yield is unstable, and the disadvantage that the purchase cost of required raw material is high is invented by long-term research and development
A kind of new preparation method has established good technical foundation to overcome the shortcomings of prior art for later industrial production.
The technical scheme is that：
1821 milligrams of 3,4- dimethoxybenzoic acids are added in the reactor, 40 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 3,4- dimethoxies
Base chlorobenzoyl chloride, yield 82.8%.
Specific implementation mode
Embodiment 1：The preparation of 3,4- dimethoxy-benzoyl chlorides：
1821 milligrams of 3,4- dimethoxybenzoic acids are added in the reactor, 40 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 3,4- dimethoxies
Base chlorobenzoyl chloride, yield 82.8%.
Embodiment 2：The preparation of 3,4- dimethoxy-benzoyl chlorides：
1821 milligrams of 3,4- dimethoxybenzoic acids are added in the reactor, 40 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 3,4- dimethoxies
Base chlorobenzoyl chloride, yield 83.6%.
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 3, the preparation method of 4- dimethoxy formyl chlorides, it is characterized in that：
1821 milligrams of 3,4- dimethoxybenzoic acids are added in the reactor, 40 milliliters of tetrahydrofuran are added, in stirring, in room temperature
0.5 milliliter of n,N-Dimethylformamide is added, is then stirred at room temperature 0.5 hour, 3 grams of thionyl chloride is added dropwise, then continues
It is stirred to react at room temperature 8 hours.After completion of the reaction, post-treated and purification process obtains compound 3,4- dimethoxy benzenes
Formyl chloride, yield 82.8%.
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 |
|---|---|---|---|
| CN201810875471.5A CN108794328A (en) | 2018-08-03 | 2018-08-03 | The preparation method of 3,4- dimethoxy-benzoyl chlorides |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810875471.5A CN108794328A (en) | 2018-08-03 | 2018-08-03 | The preparation method of 3,4- dimethoxy-benzoyl chlorides |
Publications (1)
| Publication Number | Publication Date |
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| CN108794328A true CN108794328A (en) | 2018-11-13 |
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| CN201810875471.5A Pending CN108794328A (en) | 2018-08-03 | 2018-08-03 | The preparation method of 3,4- dimethoxy-benzoyl chlorides |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007074386A2 (en) * | 2005-12-28 | 2007-07-05 | Bakulesh Mafatlal Khamar | A novel process for synthesis of itopride and it’s novel intermediate-n-(4-hydroxybenzyl)-3,4-dimethoxybenzamide |
| CN101675040A (en) * | 2007-05-03 | 2010-03-17 | 辉瑞有限公司 | Pyridine derivatives |
| WO2014013512A1 (en) * | 2012-07-19 | 2014-01-23 | Laurus Labs Private Limited | Improved process for preparation of 2,3-dihydroxy benzonitrile |
| CN108658892A (en) * | 2012-02-01 | 2018-10-16 | 希望之城 | Ribonucleotide reductase inhibitors |
-
2018
- 2018-08-03 CN CN201810875471.5A patent/CN108794328A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007074386A2 (en) * | 2005-12-28 | 2007-07-05 | Bakulesh Mafatlal Khamar | A novel process for synthesis of itopride and it’s novel intermediate-n-(4-hydroxybenzyl)-3,4-dimethoxybenzamide |
| CN101675040A (en) * | 2007-05-03 | 2010-03-17 | 辉瑞有限公司 | Pyridine derivatives |
| CN108658892A (en) * | 2012-02-01 | 2018-10-16 | 希望之城 | Ribonucleotide reductase inhibitors |
| WO2014013512A1 (en) * | 2012-07-19 | 2014-01-23 | Laurus Labs Private Limited | Improved process for preparation of 2,3-dihydroxy benzonitrile |
Non-Patent Citations (6)
| Title |
|---|
| JIA-QIANG WU等: "Rhodium(III)-catalyzed C-H/C-C activation sequence: vinylcyclopropanes as versatile synthons in direct C–H allylation reactions", 《CHEM. COMMUN.》 * |
| SARAH E. ST. JOHN等: "Design, synthesis, biological and structural evaluation of functionalized resveratrol analogues as inhibitors of quinone reductase 2", 《BIOORG. MED. CHEM.》 * |
| SHANG-SHI ZHANG等: "Mild Rhodium(III)-Catalyzed C−H Allylation with 4‑Vinyl-1,3-dioxolan-2-ones: Direct and Stereoselective Synthesis of (E)‑Allylic Alcohols", 《ORG. LETT.》 * |
| TING-YU ZHANG等: "Copper-Catalyzed Selective ortho-C−H/N−H Annulation of Benzamides with Arynes: Synthesis of Phenanthridinone Alkaloids", 《ORG. LETT.》 * |
| WEI-WEI JI等: "Heteroannulation enabled by a bimetallic Rh(III)/Ag(I) relay catalysis: application in the total synthesis of aristolactam BII", 《CHEM. COMMUN.》 * |
| 张正等: "酰氯化合物的制备方法研讨", 《江苏化工》 * |
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Application publication date: 20181113 |
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| WD01 | Invention patent application deemed withdrawn after publication |