CN106366045A - Method for producing 3-phenyl-5-chlorphenyl isoxazole - Google Patents
Method for producing 3-phenyl-5-chlorphenyl isoxazole Download PDFInfo
- Publication number
- CN106366045A CN106366045A CN201610764159.XA CN201610764159A CN106366045A CN 106366045 A CN106366045 A CN 106366045A CN 201610764159 A CN201610764159 A CN 201610764159A CN 106366045 A CN106366045 A CN 106366045A
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- China
- Prior art keywords
- chlorphenyl
- phenyl
- isoxazole
- weight
- parts
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D261/00—Heterocyclic compounds containing 1,2-oxazole or hydrogenated 1,2-oxazole rings
- C07D261/02—Heterocyclic compounds containing 1,2-oxazole or hydrogenated 1,2-oxazole rings not condensed with other rings
- C07D261/06—Heterocyclic compounds containing 1,2-oxazole or hydrogenated 1,2-oxazole rings not condensed with other rings having two or more double bonds between ring members or between ring members and non-ring members
- C07D261/08—Heterocyclic compounds containing 1,2-oxazole or hydrogenated 1,2-oxazole rings not condensed with other rings having two or more double bonds between ring members or between ring members and non-ring members with only hydrogen atoms, hydrocarbon or substituted hydrocarbon radicals, directly attached to ring carbon atoms
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Nitrogen And Oxygen As The Only Ring Hetero Atoms (AREA)
Abstract
The embodiment of the invention discloses a method for producing 3-phenyl-5-chlorphenyl isoxazole. The method comprises the steps of feeding 175 parts by weight of sodium hydroxide and 900 parts by weight of ethyl alcohol in a reaction kettle; cooling to be 35 DEG C, and feeding 120 parts by weight of para-nitrochloro-benzene; cooling to be 25 DEG C, and dropwise adding 100 parts by weight of benzyl cyanide; carrying out the thermal insulation at the temperature to be 25 to 35 DEG C for 2.5h; adding 1000 parts by weight of water, cooling to be 25 DEG C, and centrifuging and water washing to obtain a finished product. By applying the embodiment of the invention, the method has the following beneficial effects that the method for producing the 3-phenyl-5-chlorphenyl isoxazole not only uses the benzyl cyanide, the para-nitrochloro-benzene and the ethyl alcohol, but also uses cheaper sodium hydroxide, so that the production cost can be reduced, in addition, the yield of the production method is higher, and the yield of the production method provided by the invention is the highest compared with the yield of other production methods under the condition that raw meterials are with the same price.
Description
Technical field
The present invention relates to the production method of chemical substance, more particularly, to a kind of 3- phenyl -5- chlorphenyl isoxazole that produces
Method.
Background technology
3- phenyl -5- chlorphenyl isoxazole, as a kind of medicine intermediate, produces costly.Raw material therein includes benzene
Eyeball, para-nitrochloro-benzene, ethanol etc., and how to reduce its cost of material and then become the Main way of research.
Content of the invention
Embodiment of the present invention technical problem to be solved is, for the life of existing 3- phenyl -5- chlorphenyl isoxazole
Produce costly, the high problem of cost of material is it is proposed that a kind of method producing 3- phenyl -5- chlorphenyl isoxazole.
In order to solve above-mentioned technical problem, embodiments provide a kind of production 3- phenyl -5- chlorphenyl isoxazole
Method, the method for this production 3- phenyl -5- chlorphenyl isoxazole includes: put into sodium hydroxide 175 weight portion in a kettle.,
Ethanol 900 weight portion；It is cooled to 35 degrees Celsius of input para-nitrochloro-benzene 120 weight portions；It is cooled to 25 degrees Celsius of Deca benzene
Eyeball 100 weight portion；25 to 35 degrees Celsius of temperature control, is incubated 2.5 hours；Add water 1000 weight portions, 25 degrees Celsius of centrifugation washings of cooling
Draw finished product.
Wherein, ethanol is ethanol solution more than 98% for the concentration.
Implement the embodiment of the present invention, have the advantages that the production 3- phenyl -5- chlorphenyl isoxazole of the present invention
In method in addition to using benzene eyeball, para-nitrochloro-benzene, ethanol, employ relatively inexpensive sodium hydroxide, therefore, it is possible to
Reduce production cost, and, the yield rate of this kind of production method is higher, with respect to other production methods, the raw material of the same price
The finished product highest produced.
Brief description
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
Have technology description in required use accompanying drawing be briefly described it should be apparent that, drawings in the following description be only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, acceptable
Other accompanying drawings are obtained according to these accompanying drawings.
Fig. 1 is the flow chart of the method for production 3- phenyl -5- chlorphenyl isoxazole of first embodiment of the invention.
Specific embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation description is it is clear that described embodiment is only a part of embodiment of the present invention, rather than whole embodiments.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of not making creative work
Embodiment, broadly falls into the scope of protection of the invention.
Refer to Fig. 1, Fig. 1 is the stream of the method for production 3- phenyl -5- chlorphenyl isoxazole of first embodiment of the invention
Cheng Tu.In the present embodiment, the method producing 3- phenyl -5- chlorphenyl isoxazole includes:
In step s11, put into sodium hydroxide 175 weight portion, ethanol 900 weight portion in a kettle..Wherein, ethanol is
Ethanol solution more than 98% for the concentration.
In step s12, it is cooled to 35 degrees Celsius of input para-nitrochloro-benzene 120 weight portions.
In step s13, it is cooled to 25 degrees Celsius of Deca benzene eyeball 100 weight portion.
In step s14,25 to 35 degrees Celsius of temperature control, it is incubated 2.5 hours.
In step s15, add water 1000 weight portions, and 25 degrees Celsius of centrifugation washings of cooling draw finished product.
Implement the embodiment of the present invention, have the advantages that the production 3- phenyl -5- chlorphenyl isoxazole of the present invention
In method in addition to using benzene eyeball, para-nitrochloro-benzene, ethanol, employ relatively inexpensive sodium hydroxide, therefore, it is possible to
Reduce production cost, and, the yield rate of this kind of production method is higher, with respect to other production methods, the raw material of the same price
The finished product highest produced.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Within god and principle, any modification, equivalent substitution and improvement made etc., should be included within the scope of the present invention.
Claims (2)
1. a kind of method producing 3- phenyl -5- chlorphenyl isoxazole is it is characterised in that described production 3- phenyl -5- chlorphenyl
The method of isoxazole includes:
Put into sodium hydroxide 175 weight portion, ethanol 900 weight portion in a kettle.；
It is cooled to 35 degrees Celsius of input para-nitrochloro-benzene 120 weight portions；
It is cooled to 25 degrees Celsius of Deca benzene eyeball 100 weight portion；
25 to 35 degrees Celsius of temperature control, is incubated 2.5 hours；
Add water 1000 weight portions, and 25 degrees Celsius of centrifugation washings of cooling draw finished product.
2. the method for production 3- phenyl -5- chlorphenyl isoxazole according to claim 1 is it is characterised in that described ethanol
For ethanol solution more than 98% for the concentration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610764159.XA CN106366045A (en) | 2016-08-30 | 2016-08-30 | Method for producing 3-phenyl-5-chlorphenyl isoxazole |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610764159.XA CN106366045A (en) | 2016-08-30 | 2016-08-30 | Method for producing 3-phenyl-5-chlorphenyl isoxazole |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106366045A true CN106366045A (en) | 2017-02-01 |
Family
ID=57901121
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610764159.XA Pending CN106366045A (en) | 2016-08-30 | 2016-08-30 | Method for producing 3-phenyl-5-chlorphenyl isoxazole |
Country Status (1)
| Country | Link |
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| CN (1) | CN106366045A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116444398A (en) * | 2017-10-11 | 2023-07-18 | 浙江瑞博制药有限公司 | Preparation method of ketoprofen intermediate formula III |
-
2016
- 2016-08-30 CN CN201610764159.XA patent/CN106366045A/en active Pending
Non-Patent Citations (4)
| Title |
|---|
| JUANA M. PEREZ等: ""Synthesis of 3,5-Disubstituted Isoxazoles and Isoxazolines in Deep Eutectic Solvents"", 《SUSTAINABLE CHEM. ENG.》 * |
| ORLOV 等: ""Mechanism of Formation of 2,1-Benzisoxazoles in Reactions of Nitroarenes with Arylacetonitriles"", 《RUSSIAN JOURNAL OF ORGANIC CHEMISTRY》 * |
| 姚新建 等: ""阿普唑仑的化学合成"", 《郑州大学学报（医学版）》 * |
| 施小宁 等: ""水相中3,5-二芳基异噁唑衍生物的微波辐射合成"", 《应用化学》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116444398A (en) * | 2017-10-11 | 2023-07-18 | 浙江瑞博制药有限公司 | Preparation method of ketoprofen intermediate formula III |
| CN116444398B (en) * | 2017-10-11 | 2024-06-07 | 浙江瑞博制药有限公司 | Preparation method of ketoprofen intermediate formula III |
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| PB01 | Publication | ||
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Application publication date: 20170201 |