CN108689856A - A kind of new preparation process of 3- hydroxy-betas-nitrostyrolene - Google Patents
A kind of new preparation process of 3- hydroxy-betas-nitrostyrolene Download PDFInfo
- Publication number
- CN108689856A CN108689856A CN201810741382.1A CN201810741382A CN108689856A CN 108689856 A CN108689856 A CN 108689856A CN 201810741382 A CN201810741382 A CN 201810741382A CN 108689856 A CN108689856 A CN 108689856A
- Authority
- CN
- China
- Prior art keywords
- hydroxy
- nitrostyrolene
- betas
- added
- milligrams
- 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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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
The title of the present invention is a kind of new preparation process of 3- hydroxy-betas-nitrostyrolene.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- hydroxy-betas-nitrostyrolene.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 new of 3- hydroxy-betas-nitrostyrolene
Preparation method.
Background technology
3- hydroxy-betas-nitrostyrolene is a kind of intermediate feed of important synthesis medical product.
The preparation method yield of existing 3- hydroxy-betas-nitrostyrolene 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.
Invention content
The present invention uses a kind of new technology, not high for the preparation method yield of existing 3- hydroxy-betas-nitrostyrolene,
Synthesis technology is complicated, and yield is unstable, and the disadvantage that the purchase cost of required raw material is high has invented one by long-term research and development
The new preparation method of kind has established good technical foundation to overcome the shortcomings of prior art for later industrial production.
The technical scheme is that:
1221 milligrams of 3- hydroxy benzaldehydes are added in the reactor, 30 milliliters of methanol is added, 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 in methyl alcohol again, through filtering, vacuum drying is changed
Close object 3- hydroxy-betas-nitrostyrolene, yield 85.6%.
Specific implementation mode
Embodiment 1:The preparation of 3- hydroxy-betas-nitrostyrolene:
1221 milligrams of 3- hydroxy benzaldehydes are added in the reactor, 30 milliliters of methanol is added, 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 in methyl alcohol again, through filtering, vacuum drying is changed
Close object 3- hydroxy-betas-nitrostyrolene, yield 85.6%.
Embodiment 2:The preparation of 3- hydroxy-betas-nitrostyrolene:
1221 milligrams of 3- hydroxy benzaldehydes are added in the reactor, 30 milliliters of methanol is added, 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 in methyl alcohol again, through filtering, vacuum drying is changed
Close object 3- hydroxy-betas-nitrostyrolene, yield 86.9%.
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- hydroxy-betas-nitrostyrolene, it is characterized in that:
1221 milligrams of 3- hydroxy benzaldehydes are added in the reactor, 30 milliliters of methanol is added, 671 millis are added in stirring, in room temperature
Gram nitromethane, then stirred 20 minutes in ice bath, add 848 milligrams of ammonium acetate, be then stirred at room temperature 4 hours, react
Liquid turns yellow gradually.5 hours are stood, yellow solid is filtered out.It recrystallizes in methyl alcohol again, through filtering, vacuum drying obtains compound
3- hydroxy-betas-nitrostyrolene, yield 85.6%.
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 |
|---|---|---|---|
| CN201810741382.1A CN108689856A (en) | 2018-07-09 | 2018-07-09 | A kind of new preparation process of 3- hydroxy-betas-nitrostyrolene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810741382.1A CN108689856A (en) | 2018-07-09 | 2018-07-09 | A kind of new preparation process of 3- hydroxy-betas-nitrostyrolene |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108689856A true CN108689856A (en) | 2018-10-23 |
Family
ID=63851456
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810741382.1A Pending CN108689856A (en) | 2018-07-09 | 2018-07-09 | A kind of new preparation process of 3- hydroxy-betas-nitrostyrolene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108689856A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101337898A (en) * | 2007-07-06 | 2009-01-07 | 南京理工大学 | Method for synthesizing m-hydroxyphenylacetamide |
| WO2011047156A1 (en) * | 2009-10-15 | 2011-04-21 | Hercules Technology Management Co V, Inc. | Sepiapterin reductase inhibitors for the treatment of pain |
| CN102348675A (en) * | 2009-03-09 | 2012-02-08 | 巴斯夫欧洲公司 | Process for preparing substituted 2-nitrobiphenyls |
-
2018
- 2018-07-09 CN CN201810741382.1A patent/CN108689856A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101337898A (en) * | 2007-07-06 | 2009-01-07 | 南京理工大学 | Method for synthesizing m-hydroxyphenylacetamide |
| CN102348675A (en) * | 2009-03-09 | 2012-02-08 | 巴斯夫欧洲公司 | Process for preparing substituted 2-nitrobiphenyls |
| WO2011047156A1 (en) * | 2009-10-15 | 2011-04-21 | Hercules Technology Management Co V, Inc. | Sepiapterin reductase inhibitors for the treatment of pain |
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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 |