CN109053435A - The preparation method of 2,3- dimethoxy-benzoyl chloride - Google Patents
The preparation method of 2,3- dimethoxy-benzoyl chloride Download PDFInfo
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- CN109053435A CN109053435A CN201810875298.9A CN201810875298A CN109053435A CN 109053435 A CN109053435 A CN 109053435A CN 201810875298 A CN201810875298 A CN 201810875298A CN 109053435 A CN109053435 A CN 109053435A
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- dimethoxy
- added
- preparation
- room temperature
- benzoyl chloride
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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
Title of the invention is the preparation method of 2,3- dimethoxy-benzoyl chloride.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 2,3- dimethoxy-benzoyl chloride.The main points of the technical solution of the technical problems to be solved by the invention are the new preparation methods of one kind of the compound.
Description
Technical field
The present invention relates to pharmaceutical technology fields, specifically, the present invention relates to 2, the preparation of 3- dimethoxy-benzoyl chloride
Method.
Background technique
2,3- dimethoxy-benzoyl chlorides are a kind of intermediate feeds of important synthesis medical product.
The preparation method yield of existing 2,3- dimethoxy-benzoyl chloride is not high, and synthesis technology is complicated, and yield is unstable,
Need 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.
Summary of the invention
The present invention use a kind of new technology, for existing 2,3- dimethoxy-benzoyl chloride preparation method yield not
Height, synthesis technology is complicated, and yield is unstable, the high disadvantage of the purchase cost of required raw material, by long-term research and development, invention
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 2,3- dimethoxybenzoic acids are added in the reactor, are added 40 milliliters of tetrahydrofuran, in stirring, room
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 2,3- dimethoxy
Base chlorobenzoyl chloride, yield 81.8%.
Specific embodiment
The preparation of embodiment 1:2,3- dimethoxy-benzoyl chloride:
1821 milligrams of 2,3- dimethoxybenzoic acids are added in the reactor, are added 40 milliliters of tetrahydrofuran, in stirring, room
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 2,3- dimethoxy
Base chlorobenzoyl chloride, yield 81.8%.
The preparation of embodiment 2:2,3- dimethoxy-benzoyl chloride:
1821 milligrams of 2,3- dimethoxybenzoic acids are added in the reactor, are added 40 milliliters of tetrahydrofuran, in stirring, room
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 2,3- dimethoxy
Base chlorobenzoyl chloride, yield 82.9%.
The present invention can be summarized with others without prejudice to the concrete form of spirit or essential characteristics of the 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 preparation method of 3- dimethoxy formyl chloride, it is characterized in that:
1821 milligrams of 2,3- dimethoxybenzoic acids are added in the reactor, are added 40 milliliters of tetrahydrofuran, 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 2,3- dimethoxy benzene
Formyl chloride, yield 81.8%.
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)
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CN201810875298.9A CN109053435A (en) | 2018-08-03 | 2018-08-03 | The preparation method of 2,3- dimethoxy-benzoyl chloride |
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CN201810875298.9A CN109053435A (en) | 2018-08-03 | 2018-08-03 | The preparation method of 2,3- dimethoxy-benzoyl chloride |
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CN109053435A true CN109053435A (en) | 2018-12-21 |
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CN201810875298.9A Pending CN109053435A (en) | 2018-08-03 | 2018-08-03 | The preparation method of 2,3- dimethoxy-benzoyl chloride |
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1220660A (en) * | 1996-05-30 | 1999-06-23 | 赫彻斯特马里恩鲁斯公司 | Alkyloxyamino substituted fluorenones and their use as protein kinase cinhibitors |
WO2002070469A2 (en) * | 2001-03-05 | 2002-09-12 | Icos Corporation | Selective pde3b inhibitors and use of the same in therapy |
WO2014013512A1 (en) * | 2012-07-19 | 2014-01-23 | Laurus Labs Private Limited | Improved process for preparation of 2,3-dihydroxy benzonitrile |
-
2018
- 2018-08-03 CN CN201810875298.9A patent/CN109053435A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1220660A (en) * | 1996-05-30 | 1999-06-23 | 赫彻斯特马里恩鲁斯公司 | Alkyloxyamino substituted fluorenones and their use as protein kinase cinhibitors |
WO2002070469A2 (en) * | 2001-03-05 | 2002-09-12 | Icos Corporation | Selective pde3b inhibitors and use of the same in therapy |
WO2014013512A1 (en) * | 2012-07-19 | 2014-01-23 | Laurus Labs Private Limited | Improved process for preparation of 2,3-dihydroxy benzonitrile |
Non-Patent Citations (1)
Title |
---|
CYNTHIA M. HONG等: "Conformational Selection as the Mechanism of Guest Binding in a Flexible Supramolecular Host", 《J. AM. CHEM. SOC》 * |
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Application publication date: 20181221 |