CN108929228A - A kind of new preparation process of 3- methoxyl group-beta-nitrostyrene - Google Patents
A kind of new preparation process of 3- methoxyl group-beta-nitrostyrene Download PDFInfo
- Publication number
- CN108929228A CN108929228A CN201810741374.7A CN201810741374A CN108929228A CN 108929228 A CN108929228 A CN 108929228A CN 201810741374 A CN201810741374 A CN 201810741374A CN 108929228 A CN108929228 A CN 108929228A
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- China
- Prior art keywords
- beta
- nitrostyrene
- methoxyl group
- added
- new preparation
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/12—Preparation of nitro compounds by reactions not involving the formation of nitro groups
Abstract
Title of the invention is a kind of new preparation process of 3- methoxyl group-beta-nitrostyrene.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- methoxyl group-beta-nitrostyrene.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 a kind of 3- methoxyl group-beta-nitrostyrenes
New preparation process.
Background technique
3- methoxyl group-beta-nitrostyrene is a kind of intermediate feed of important synthesis medical product.
The preparation method yield of existing 3- methoxyl group-beta-nitrostyrene is not high, and synthesis technology is complicated, and yield is unstable
It is fixed, need to invent a kind of new preparation method, to overcome the shortcomings of prior art.
Summary of the invention
The present invention use a kind of new technology, for existing 3- methoxyl group-beta-nitrostyrene 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
1362 milligrams of m-methoxybenzaldehydes are added in the reactor, is added 30 milliliters of methanol, in stirring, is added in room temperature
Then 671 milligrams of nitromethane stirs 20 minutes in ice bath, adds 848 milligrams of ammonium acetate, is then stirred at room temperature 4 hours,
Reaction solution turns yellow gradually.5 hours are stood, yellow solid is filtered out.It recrystallizes, is filtered in methyl alcohol again, be dried in vacuo, changed
Close object 3- methoxyl group-beta-nitrostyrene, yield 87.7%.
Specific embodiment
The preparation of embodiment 1:3- methoxyl group-beta-nitrostyrene:
1362 milligrams of m-methoxybenzaldehydes are added in the reactor, is added 30 milliliters of methanol, in stirring, is added in room temperature
Then 671 milligrams of nitromethane stirs 20 minutes in ice bath, adds 848 milligrams of ammonium acetate, is then stirred at room temperature 4 hours,
Reaction solution turns yellow gradually.5 hours are stood, yellow solid is filtered out.It recrystallizes, is filtered in methyl alcohol again, be dried in vacuo, changed
Close object 3- methoxyl group-beta-nitrostyrene, yield 90.2%.
The preparation of embodiment 2:3- methoxyl group-beta-nitrostyrene:
1362 milligrams of m-methoxybenzaldehydes are added in the reactor, is added 30 milliliters of methanol, in stirring, is added in room temperature
Then 671 milligrams of nitromethane stirs 20 minutes in ice bath, adds 848 milligrams of ammonium acetate, is then stirred at room temperature 4 hours,
Reaction solution turns yellow gradually.5 hours are stood, yellow solid is filtered out.It recrystallizes, is filtered in methyl alcohol again, be dried in vacuo, changed
Close object 3- methoxyl group-beta-nitrostyrene, yield 87.7%.
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. a kind of new preparation process of 3- methoxyl group-beta-nitrostyrene, it is characterized in that:
1362 milligrams of m-methoxybenzaldehydes are added in the reactor, is added 30 milliliters of methanol, in stirring, 671 is added in room temperature
The nitromethane of milligram, then stirs 20 minutes in ice bath, adds 848 milligrams of ammonium acetate, is then stirred at room temperature 4 hours, instead
Liquid is answered to turn yellow gradually.5 hours are stood, yellow solid is filtered out.It recrystallizes, is filtered in methyl alcohol again, be dried in vacuo, obtain chemical combination
Object 3- methoxyl group-beta-nitrostyrene, yield 87.7%.
2. according to the method described in claim 1, it is characterized in that:
It needs that compounds acetic acid ammonium is added in reaction solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810741374.7A CN108929228A (en) | 2018-07-09 | 2018-07-09 | A kind of new preparation process of 3- methoxyl group-beta-nitrostyrene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810741374.7A CN108929228A (en) | 2018-07-09 | 2018-07-09 | A kind of new preparation process of 3- methoxyl group-beta-nitrostyrene |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108929228A true CN108929228A (en) | 2018-12-04 |
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ID=64447511
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810741374.7A Pending CN108929228A (en) | 2018-07-09 | 2018-07-09 | A kind of new preparation process of 3- methoxyl group-beta-nitrostyrene |
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| CN (1) | CN108929228A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000021947A1 (en) * | 1998-10-15 | 2000-04-20 | Zambon Group S.P.A. | Benzazine derivatives as phosphodiesterase 4 inhibitors |
| WO2011006000A1 (en) * | 2009-07-08 | 2011-01-13 | Haiyan Liu | Berberine derivatives useful for modulating lipid levels and their methods of synthesis |
| CN102348675A (en) * | 2009-03-09 | 2012-02-08 | 巴斯夫欧洲公司 | Process for preparing substituted 2-nitrobiphenyls |
| CN103108871A (en) * | 2010-09-16 | 2013-05-15 | 诺瓦提斯公司 | 17a-hydroxylase/c17,20-lyase inhibitors |
-
2018
- 2018-07-09 CN CN201810741374.7A patent/CN108929228A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000021947A1 (en) * | 1998-10-15 | 2000-04-20 | Zambon Group S.P.A. | Benzazine derivatives as phosphodiesterase 4 inhibitors |
| CN102348675A (en) * | 2009-03-09 | 2012-02-08 | 巴斯夫欧洲公司 | Process for preparing substituted 2-nitrobiphenyls |
| WO2011006000A1 (en) * | 2009-07-08 | 2011-01-13 | Haiyan Liu | Berberine derivatives useful for modulating lipid levels and their methods of synthesis |
| CN103108871A (en) * | 2010-09-16 | 2013-05-15 | 诺瓦提斯公司 | 17a-hydroxylase/c17,20-lyase inhibitors |
Non-Patent Citations (1)
| Title |
|---|
| ANDRZEJ J. BOJARSKI等: "The Influence of Substitution at Aromatic Part of 1,2,3,4-Tetrahy -droisoquinoline on In Vitro and In Vivo 5-HT1A/5-HT2A Receptor Activities of Its 1-Adamantoyloaminoalkyl Derivatives", 《BIOORGANIC & MEDICINAL CHEMISTRY》 * |
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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 | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20181204 |