CN103804164A - Preparation method of 4,4'-difluoro diphenylmethanone - Google Patents
Preparation method of 4,4'-difluoro diphenylmethanone Download PDFInfo
- Publication number
- CN103804164A CN103804164A CN201210441920.8A CN201210441920A CN103804164A CN 103804164 A CN103804164 A CN 103804164A CN 201210441920 A CN201210441920 A CN 201210441920A CN 103804164 A CN103804164 A CN 103804164A
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- preparation
- solution
- fluorobenzene
- difluoro
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/093—Preparation of halogenated hydrocarbons by replacement by halogens
- C07C17/10—Preparation of halogenated hydrocarbons by replacement by halogens of hydrogen atoms
- C07C17/14—Preparation of halogenated hydrocarbons by replacement by halogens of hydrogen atoms in the side-chain of aromatic compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/45—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by condensation
- C07C45/46—Friedel-Crafts reactions
-
- 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
Abstract
The invention discloses a preparation method of 4,4'-difluoro diphenylmethanone. The preparation method comprises following steps: chlorine is added into a 4-fluorotoluene solution, and benzoyl peroxide is used so as to realize chlorination of an obtained mixture at a temperature of 150 to 250 DEG C; excess aluminium trichloride is added into the chloridized mixture, and the chloridized mixture is reacted for 1 to 2h at a constant temperature of 80 to 120 DEG C; fluorobenzene is added into an obtained reaction product, and an obtained mixed material is subjected to distillation under a pressure of -0.85MPa, wherein the mole ratio of 4-fluorotoluene to fluorobenzene is 2-2.5:1; active carbon and ethanol are added, and an obtained product is subjected to crystallization, and filtration so as to obtain 4,4'-difluoro diphenylmethanone. Reaction conditions of the preparation method are easy to control; yield is high; the preparation method is suitable for industrialized production; no pollution on equipment and the environment is caused by the reaction, and safety in use is high.
Description
Technical field
The present invention relates to one 4, the preparation technology of 4 '-difluoro benzophenone.
Background technology
In chemical industry technical field, 4,4 '-difluoro benzophenone, as a kind of engineering plastics of high temperature resistant, burn into friction, is widely used.Tradition 4, the preparation of 4 '-difluoro benzophenone roughly has three kinds: Fu Shi alkylation process, diazotization method and halogen exchange are sent out, and above-mentioned three kinds of preparation method's reaction conditionss restriction is strict, serious to equipment and environmental pollution, and there is potential safety hazard, be not suitable for industrialized production and promote.
Summary of the invention
For deficiency of the prior art, the invention provides that a kind of processing requirement is simple, productive rate is high, non-environmental-pollution, be applicable to 4 of suitability for industrialized production, the preparation technology of 4 '-difluoro benzophenone.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is: one 4, and the preparation technology of 4 '-difluoro benzophenone, is characterized in that: logical chlorine in 4-toluene fluoride solution, select Benzoyl Peroxide to make solution chlorination at 150-250 ℃; In the solution after chlorination, add excessive aluminum chloride, react 1-2h at constant temperature 80-120 ℃; In the most backward solution, add fluorobenzene, 4-toluene fluoride and fluorobenzene mol ratio are 2-2.5: 1, decompression-0.85MPa distillation, adds gac and ethanol, crystallization, filter 4,4 '-difluoro benzophenone.
The present invention directly adopts 4-toluene fluoride to carry out chlorination, hydrolysis, condensation, logical fluorobenzene underpressure distillation, crystallization, filter 4,4 '-difluoro benzophenone finished product, its easily-controlled reaction conditions, productive rate is high, is applicable to suitability for industrialized production, and reaction is to equipment and environmental nonpollution, and usage safety performance is high.
Embodiment
Below further illustrate the specific embodiment of the present invention.
Embodiment mono-:
One 4, the preparation technology of 4 '-difluoro benzophenone, in 4-toluene fluoride solution, logical chlorine, selects Benzoyl Peroxide to make solution chlorination at 150 ℃; In the solution after chlorination, add excessive aluminum chloride, at 80 ℃ of constant temperature, react 1h; In the most backward solution, add fluorobenzene, 4-toluene fluoride and fluorobenzene mol ratio are 2: 1, and decompression-0.85MPa distillation adds gac and ethanol, crystallization, filter 4,4 '-difluoro benzophenone.
Embodiment bis-:
One 4, the preparation technology of 4 '-difluoro benzophenone, in 4-toluene fluoride solution, logical chlorine, selects Benzoyl Peroxide to make solution chlorination at 200 ℃; In the solution after chlorination, add excessive aluminum chloride, at 100 ℃ of constant temperature, react 1.5h; In the most backward solution, add fluorobenzene, 4-toluene fluoride and fluorobenzene mol ratio are 2.3: 1, and decompression-0.85MPa distillation adds gac and ethanol, crystallization, filter 4,4 '-difluoro benzophenone.
Embodiment tri-:
One 4, the preparation technology of 4 '-difluoro benzophenone, in 4-toluene fluoride solution, logical chlorine, selects Benzoyl Peroxide to make solution chlorination at 250 ℃; In the solution after chlorination, add excessive aluminum chloride, at 120 ℃ of constant temperature, react 2h; In the most backward solution, add fluorobenzene, 4-toluene fluoride and fluorobenzene mol ratio are 2.5: 1, and decompression-0.85MPa distillation adds gac and ethanol, crystallization, filter to obtain 4,4 ' one difluoro benzophenone.
Claims (2)
1. one kind 4, the preparation technology of 4 '-difluoro benzophenone, is characterized in that: logical chlorine in 4-toluene fluoride solution, and select Benzoyl Peroxide to make solution chlorination at 150-250 ℃; In the solution after chlorination, add excessive aluminum chloride, react 1-2h at constant temperature 80-120 ℃; In the most backward solution, add fluorobenzene, decompression-0.85MPa distillation, add gac and ethanol, crystallization, filter 4,4 '-difluoro benzophenone.
2. according to claim 1 a kind of 4, the preparation technology of 4 '-difluoro benzophenone, is characterized in that: 4-toluene fluoride and fluorobenzene mol ratio are 2-2.5: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210441920.8A CN103804164A (en) | 2012-11-07 | 2012-11-07 | Preparation method of 4,4'-difluoro diphenylmethanone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210441920.8A CN103804164A (en) | 2012-11-07 | 2012-11-07 | Preparation method of 4,4'-difluoro diphenylmethanone |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103804164A true CN103804164A (en) | 2014-05-21 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210441920.8A Pending CN103804164A (en) | 2012-11-07 | 2012-11-07 | Preparation method of 4,4'-difluoro diphenylmethanone |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103804164A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108610245A (en) * | 2018-05-22 | 2018-10-02 | 江苏万隆化学有限公司 | A kind of preparation method of high-purity difluoro benzophenone |
| CN110872216A (en) * | 2019-12-06 | 2020-03-10 | 南京恒道医药科技有限公司 | Method and device for producing (2-chloro-5-iodophenyl) -4-fluorobenzyl ketone by reaction separation coupling |
-
2012
- 2012-11-07 CN CN201210441920.8A patent/CN103804164A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108610245A (en) * | 2018-05-22 | 2018-10-02 | 江苏万隆化学有限公司 | A kind of preparation method of high-purity difluoro benzophenone |
| CN110872216A (en) * | 2019-12-06 | 2020-03-10 | 南京恒道医药科技有限公司 | Method and device for producing (2-chloro-5-iodophenyl) -4-fluorobenzyl ketone by reaction separation coupling |
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| Date | Code | Title | Description |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20140521 |