CN108238870A - A kind of synthetic method of medical material Hexafluoro acetone - Google Patents
A kind of synthetic method of medical material Hexafluoro acetone Download PDFInfo
- Publication number
- CN108238870A CN108238870A CN201710215443.6A CN201710215443A CN108238870A CN 108238870 A CN108238870 A CN 108238870A CN 201710215443 A CN201710215443 A CN 201710215443A CN 108238870 A CN108238870 A CN 108238870A
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- China
- Prior art keywords
- solution
- hexafluoro
- synthetic method
- medical material
- hexafluoro acetone
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- 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
- C07C45/51—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by pyrolysis, rearrangement or decomposition
- C07C45/511—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by pyrolysis, rearrangement or decomposition involving transformation of singly bound oxygen functional groups to >C = O groups
- C07C45/512—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by pyrolysis, rearrangement or decomposition involving transformation of singly bound oxygen functional groups to >C = O groups the singly bound functional group being a free hydroxyl group
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A kind of synthetic method of medical material Hexafluoro acetone, mainly includes the following steps：2, the 3 dihydroxy hexafluoro isopentane of 3mol, the N methyl propanamide solution of 4 6mol are added in reaction vessel, solution temperature is increased to 70 80 DEG C, keeps 60 80min, then adds in the bismuth molybdate of 2 3mol, the reaction was continued 50 70min, temperature is reduced to 40 50 DEG C, vacuum distillation, the fraction of 80-89 DEG C of collection, m-cresol solution washs, m-chloroaniline solution washs, and methoxy methyl benzole soln recrystallization obtains crystal Hexafluoro acetone.
Description
Technical field
The present invention relates to a kind of synthetic methods of medical material Hexafluoro acetone.
Background technology
Hexafluoro acetone is mainly used as organic solvent, and high temperature resistant, corrosion resistant coating and adhesion are can obtain with the copolymerization of ring chloroethanes
Agent is the raw material for synthesizing medicine, pesticide, high molecular material and organic chemicals.But existing synthetic method is mostly using complete
Fluorine isobutene and potassium permanganate reaction synthesis, process is more complicated, and ultimate yield is simultaneously not bery high, therefore, it is necessary to propose one kind
New synthetic method, this quality and yield for further improving product, reducing by-products content has important economic meaning
Justice.
Invention content
The purpose of the present invention is to provide a kind of synthetic methods of medical material Hexafluoro acetone, include the following steps：
(i) 2,3- dihydroxy-hexafluoro isopentane of 3mol is added in reaction vessel, the N- methyl propanamides of 4-6mol are molten
Liquid, raising solution temperature keep 60-80min to 70-80 DEG C, then add in the bismuth molybdate of 2-3mol, the reaction was continued 50-
70min reduces temperature to 40-50 DEG C, vacuum distillation, collects 80-89 DEG C of fraction, and m-cresol solution washs, and m-chloroaniline is molten
Liquid washs, and methoxy methyl benzole soln recrystallization obtains crystal Hexafluoro acetone；Wherein, the N- methyl propanamide solution described in step (i)
Mass fraction is 60-68%, and pressure residing for the vacuum distillation described in step (i) is 10-20kPa, described in step (i) between first
Phenol solution mass fraction is 70-76%, and the m-chloroaniline liquid quality fraction described in step (i) is 80-85%, step (i)
The methoxy toluene liquid quality fraction is 92-96%.
Entire reaction process can be represented with following reaction formula：
The invention has the advantages that：Reduce the intermediate link of reaction, shorten the reaction time, improve reaction yield.
Specific embodiment
With reference to specific implementation example, the invention will be further described：
Example 1：
2,3- dihydroxy-hexafluoro isopentane of 3mol is added in reaction vessel, 4mol mass fractions are 60% N- first
Base propionyl amine aqueous solution, raising solution temperature keep 60min to 70 DEG C, then add in the bismuth molybdate of 2mol, the reaction was continued 50min,
Temperature is reduced to 40 DEG C, residing pressure is evaporated under reduced pressure for 10kPa, collects 80 DEG C of fraction, and mass fraction is 70% metacresol
Solution washs, and the m-chloroaniline solution that mass fraction is 80% washs, and the methoxy methyl benzole soln that mass fraction is 92% is tied again
Crystalline substance obtains crystal Hexafluoro acetone 478.08g, yield 96%.
Example 2：
2,3- dihydroxy-hexafluoro isopentane of 3mol is added in reaction vessel, 5mol mass fractions are 65% N- first
Base propionyl amine aqueous solution, raising solution temperature keep 70min to 75 DEG C, then add in the bismuth molybdate of 2.5mol, the reaction was continued
60min reduces temperature to 45 DEG C, and 15kPa vacuum distillations, the fraction of 85 DEG C of collection, mass fraction is 73% m-cresol solution
Washing, the m-chloroaniline solution that mass fraction is 82% wash, and the methoxy methyl benzole soln that mass fraction is 93% recrystallizes, and obtains
Crystal Hexafluoro acetone 483.06g, yield 97%.
Example 3：
2,3- dihydroxy-hexafluoro isopentane of 3mol is added in reaction vessel, 6mol mass fractions are 68% N- first
Base propionyl amine aqueous solution, raising solution temperature keep 80min to 80 DEG C, then add in the bismuth molybdate of 3mol, the reaction was continued 70min,
Temperature is reduced to 50 DEG C, 20kPa is evaporated under reduced pressure, and collects 89 DEG C of fraction, and the m-cresol solution that mass fraction is 76% washs, matter
It measures the m-chloroaniline solution that score is 85% to wash, the methoxy methyl benzole soln that mass fraction is 96% recrystallizes, and obtains crystal six
Fluorine acetone 490.53g, yield 98.5%.
Claims (3)
1. a kind of synthetic method of medical material Hexafluoro acetone, which is characterized in that mainly include the following steps：(i) hold in reaction
2,3- dihydroxy-hexafluoro isopentane of 3mol is added in device, the N- methyl propanamide solution of 4-6mol, raising solution temperature is extremely
70-80 DEG C, 60-80min is kept, then adds in the bismuth molybdate of 2-3mol, the reaction was continued 50-70min, reduction temperature to 40-50
DEG C, vacuum distillation, the fraction of 80-89 DEG C of collection, m-cresol solution washing, the washing of m-chloroaniline solution, methoxy methyl benzole soln
Recrystallization, obtains crystal Hexafluoro acetone；Wherein, the N- methyl propanamides liquid quality fraction described in step (i) is 60-68%, step
Suddenly pressure residing for the vacuum distillation described in (i) is 10-20kPa, m-cresol solution mass fraction described in step (i) for 70-
76%.
2. a kind of synthetic method of medical material Hexafluoro acetone according to claim 1, which is characterized in that step (i) is described
M-chloroaniline liquid quality fraction be 80-85%.
3. a kind of synthetic method of medical material Hexafluoro acetone according to claim 1, which is characterized in that step (i) is described
Methoxy toluene liquid quality fraction be 92-96%.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710215443.6A CN108238870A (en) | 2017-04-05 | 2017-04-05 | A kind of synthetic method of medical material Hexafluoro acetone |
| GBGB1705850.4A GB201705850D0 (en) | 2017-04-05 | 2017-04-11 | Pharmaceutical raw materials hexafluoroacetone synthesis method |
| IES20180078A IES86972B2 (en) | 2017-04-05 | 2018-03-27 | Pharmaceutical raw materials hexafluoroacetone synthesis method |
| AU2018100416A AU2018100416A4 (en) | 2017-04-05 | 2018-04-01 | Pharmaceutical raw materials hexafluoroacetone synthesis method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710215443.6A CN108238870A (en) | 2017-04-05 | 2017-04-05 | A kind of synthetic method of medical material Hexafluoro acetone |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108238870A true CN108238870A (en) | 2018-07-03 |
Family
ID=58744602
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710215443.6A Pending CN108238870A (en) | 2017-04-05 | 2017-04-05 | A kind of synthetic method of medical material Hexafluoro acetone |
Country Status (4)
| Country | Link |
|---|---|
| CN (1) | CN108238870A (en) |
| AU (1) | AU2018100416A4 (en) |
| GB (1) | GB201705850D0 (en) |
| IE (1) | IES86972B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113527975A (en) * | 2021-07-28 | 2021-10-22 | 上海涂固安高科技有限公司 | Water-based fluorine-containing coating and preparation method thereof |
-
2017
- 2017-04-05 CN CN201710215443.6A patent/CN108238870A/en active Pending
- 2017-04-11 GB GBGB1705850.4A patent/GB201705850D0/en not_active Ceased
-
2018
- 2018-03-27 IE IES20180078A patent/IES86972B2/en unknown
- 2018-04-01 AU AU2018100416A patent/AU2018100416A4/en not_active Ceased
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113527975A (en) * | 2021-07-28 | 2021-10-22 | 上海涂固安高科技有限公司 | Water-based fluorine-containing coating and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| IES86972B2 (en) | 2019-05-01 |
| IES20180078A2 (en) | 2019-04-03 |
| AU2018100416A4 (en) | 2018-05-10 |
| GB201705850D0 (en) | 2017-05-24 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180703 |