CN108863768A - The preparation method of 3,5- dimethoxy-benzoyl chloride - Google Patents
The preparation method of 3,5- dimethoxy-benzoyl chloride Download PDFInfo
- Publication number
- CN108863768A CN108863768A CN201810875546.XA CN201810875546A CN108863768A CN 108863768 A CN108863768 A CN 108863768A CN 201810875546 A CN201810875546 A CN 201810875546A CN 108863768 A CN108863768 A CN 108863768A
- Authority
- CN
- China
- Prior art keywords
- added
- dimethoxy
- preparation
- room temperature
- benzoyl chloride
- 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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Links
- 238000002360 preparation method Methods 0.000 title claims abstract 5
- FTHPLWDYWAKYCY-UHFFFAOYSA-N 3,5-dimethoxybenzoyl chloride Chemical compound COC1=CC(OC)=CC(C(Cl)=O)=C1 FTHPLWDYWAKYCY-UHFFFAOYSA-N 0.000 title abstract 3
- 150000001875 compounds Chemical class 0.000 claims abstract 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims 3
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims 2
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims 2
- IWPZKOJSYQZABD-UHFFFAOYSA-N 3,5-dimethoxybenzoic acid Chemical class COC1=CC(OC)=CC(C(O)=O)=C1 IWPZKOJSYQZABD-UHFFFAOYSA-N 0.000 claims 1
- -1 compound 3,5- dimethoxy benzene Formyl chloride Chemical class 0.000 claims 1
- 238000000034 method Methods 0.000 claims 1
- 238000000746 purification Methods 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims 1
Classifications
-
- 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
Title of the invention is the preparation method of 3,5- 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 3,5- 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 3, the preparation of 5- dimethoxy-benzoyl chloride
Method.
Background technique
3,5- dimethoxy-benzoyl chlorides are a kind of intermediate feeds of important synthesis medical product.
The preparation method yield of existing 3,5- 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 3,5- 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 3,5- dimethoxybenzoic acids are added in the reactor, are added 40 milliliters of tetrahydrofuran, in stirring,
0.5 milliliter of n,N-Dimethylformamide is added in room temperature, is then stirred at room temperature 0.5 hour, 3 grams of thionyl chloride is added dropwise, so
After continue to be stirred to react at room temperature 8 hours.After completion of the reaction, post-treated and purification process obtains compound 3,5- diformazan
Oxygroup chlorobenzoyl chloride, yield 77.9%.
Specific embodiment
Embodiment 1：The preparation of 3,5- dimethoxy-benzoyl chlorides：
1821 milligrams of 3,5- dimethoxybenzoic acids are added in the reactor, are added 40 milliliters of tetrahydrofuran, in stirring,
0.5 milliliter of n,N-Dimethylformamide is added in room temperature, is then stirred at room temperature 0.5 hour, 3 grams of thionyl chloride is added dropwise, so
After continue to be stirred to react at room temperature 8 hours.After completion of the reaction, post-treated and purification process obtains compound 3,5- diformazan
Oxygroup chlorobenzoyl chloride, yield 79.5%.
Embodiment 2：The preparation of 3,5- dimethoxy-benzoyl chloride：
1821 milligrams of 3,5- dimethoxybenzoic acids are added in the reactor, are added 40 milliliters of tetrahydrofuran, in stirring,
0.5 milliliter of n,N-Dimethylformamide is added in room temperature, is then stirred at room temperature 0.5 hour, 3 grams of thionyl chloride is added dropwise, so
After continue to be stirred to react at room temperature 8 hours.After completion of the reaction, post-treated and purification process obtains compound 3,5- diformazan
Oxygroup chlorobenzoyl chloride, yield 83.6%.
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)
- The preparation method of 1.3,5- dimethoxy formyl chlorides, it is characterized in that：1821 milligrams of 3,5- 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 3,5- dimethoxy benzene Formyl chloride, yield 77.9%.
- 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 |
|---|---|---|---|
| CN201810875546.XA CN108863768A (en) | 2018-08-03 | 2018-08-03 | The preparation method of 3,5- dimethoxy-benzoyl chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810875546.XA CN108863768A (en) | 2018-08-03 | 2018-08-03 | The preparation method of 3,5- dimethoxy-benzoyl chloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108863768A true CN108863768A (en) | 2018-11-23 |
Family
ID=64307223
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810875546.XA Pending CN108863768A (en) | 2018-08-03 | 2018-08-03 | The preparation method of 3,5- dimethoxy-benzoyl chloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108863768A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014013512A1 (en) * | 2012-07-19 | 2014-01-23 | Laurus Labs Private Limited | Improved process for preparation of 2,3-dihydroxy benzonitrile |
| WO2016091789A1 (en) * | 2014-12-09 | 2016-06-16 | Consejo Superior De Investigaciones Cientificas | DERIVATIVES OF 2-PHENYL-7,7a-DIHYDRO-3aH-PYRANO[3,4-d]OXAZOLE-6(4H)-ONE |
| CN108137526A (en) * | 2015-07-10 | 2018-06-08 | 诺拉姆科有限公司 | For producing the method for cannabidiol and △ -9- tetrahydrocannabinol |
-
2018
- 2018-08-03 CN CN201810875546.XA patent/CN108863768A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014013512A1 (en) * | 2012-07-19 | 2014-01-23 | Laurus Labs Private Limited | Improved process for preparation of 2,3-dihydroxy benzonitrile |
| WO2016091789A1 (en) * | 2014-12-09 | 2016-06-16 | Consejo Superior De Investigaciones Cientificas | DERIVATIVES OF 2-PHENYL-7,7a-DIHYDRO-3aH-PYRANO[3,4-d]OXAZOLE-6(4H)-ONE |
| CN108137526A (en) * | 2015-07-10 | 2018-06-08 | 诺拉姆科有限公司 | For producing the method for cannabidiol and △ -9- tetrahydrocannabinol |
Non-Patent Citations (4)
| Title |
|---|
| E. S. KELBYSHEVA等: "Dicarbonyl chelates from 1-cymantrenylalkylamides with the dendrite structure：formation，photochromism，and kinetics of dark reaction with carbon monoxide", 《RUSSIAN CHEMICAL BULLETIN》 * |
| M. DAMODER REDDY等: "Palladium-Catalyzed，N-(2-Aminophenyl)acetamide-Assisted Ortho-Arylation of Substituted Benzamides：Application to the Synthesis of Urolithins B, M6, and M7", 《J. ORG. CHEM.》 * |
| SARAH E. ST. JOHN等: "Design，synthesis，biological and structural evaluation of functionalized resveratrol analogues as inhibitors of quinone reductase 2", 《BIOORG. MED. CHEM.》 * |
| 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: 20181123 |
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