CN107285990A - A kind of preparation method of 2,7 dichloro fluorenes - Google Patents
A kind of preparation method of 2,7 dichloro fluorenes Download PDFInfo
- Publication number
- CN107285990A CN107285990A CN201710530237.4A CN201710530237A CN107285990A CN 107285990 A CN107285990 A CN 107285990A CN 201710530237 A CN201710530237 A CN 201710530237A CN 107285990 A CN107285990 A CN 107285990A
- Authority
- CN
- China
- Prior art keywords
- fluorenes
- chlorine
- dichloro
- preparation
- glacial acetic
- 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
- 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
- C07C17/12—Preparation of halogenated hydrocarbons by replacement by halogens of hydrogen atoms in the ring of aromatic compounds
Abstract
The present invention relates to a kind of preparation method of 2,7 dichloro fluorenes, comprise the following steps：(1) 200g fluorenes, 400 600ml glacial acetic acids, 0.2g anhydrous ferric trichlorides are added in reactor, temperature is increased to 20 DEG C；Appropriate chlorine is passed through, sampling detection when HPLC detects chlorine fluorenes purity≤5% of reaction intermediate one, stops logical chlorine, continues to stir 10 minutes；90 DEG C are warming up to, is stirred 1 hour, cooling, suction filtration is washed with a small amount, dries, obtains 2,7 dichloro fluorenes.
Description
Technical field
The present invention relates to the preparation method of one kind 2,7- dichloro fluorenes, belong to field of medicine and chemical technology.
Background technology
LUMEFANTRINE is a kind of common, effective anti-malaria medicaments, and 2,7- dichloro fluorenes are the important centres for preparing LUMEFANTRINE
Body, current 2,7- dichloros fluorenes cooks chlorinating agent in the glacial acetic acid in 10 times of volumes with chlorine, and ferric trichloride is catalyst preparation
Form, yield only has 30-35%, yield is relatively low.
The content of the invention
It is an object of the invention to provide the preparation method of one kind 2,7- dichloro fluorenes, the ratio of adjustment glacial acetic acid and raw material fluorenes,
And reaction temperature is improved in the later stage, to lift the yield of product.
To achieve the above object, the technical scheme is that：
The preparation method of one kind 2,7- dichloro fluorenes, comprises the following steps：
(1) 200g fluorenes, 400-600ml glacial acetic acids, 0.2g anhydrous ferric trichlorides are added in reactor, temperature is increased to 20
℃；
(2) appropriate chlorine is passed through, sampling detection, when HPLC detects chlorine fluorenes purity≤5% of reaction intermediate one, stops logical
Chlorine, continues to stir 10 minutes；
(3) 90 DEG C are warming up to, is stirred 1 hour, cooling, suction filtration is washed with a small amount, dries, obtains 2,7- dichloro fluorenes.
As further preferably, the preparation method of one kind 2,7- dichloro fluorenes comprises the following steps：
(1) 200g fluorenes, 500ml glacial acetic acids, 0.2g anhydrous ferric trichlorides are added in reactor, temperature is increased to 20 DEG C；
(2) appropriate chlorine is passed through, sampling detection, when HPLC detects chlorine fluorenes purity≤5% of reaction intermediate one, stops logical
Chlorine, continues to stir 10 minutes；
(3) 90 DEG C are warming up to, is stirred 1 hour, cooling, suction filtration is washed with a small amount, dries, obtains 2,7- dichloro fluorenes.
The preparation method of one kind 2,7- dichloro fluorenes of the invention, by adjusting the ratio of glacial acetic acid and raw material fluorenes, and in the later stage
Reaction temperature is improved, the yield of product is substantially improved.
Embodiment
Following embodiment, is merely illustrative of, and is not only, so, all within the scope of the present invention or make with
The similar change of the present invention is both contained within the present invention.
Embodiment 1：
The preparation method of one kind 2,7- dichloro fluorenes, comprises the following steps：
(1) 200g fluorenes, 400ml glacial acetic acids, 0.2g anhydrous ferric trichlorides are added in reactor, temperature is increased to 20 DEG C；
(2) appropriate chlorine is passed through, sampling detection, when HPLC detects chlorine fluorenes purity≤5% of reaction intermediate one, stops logical
Chlorine, continues to stir 10 minutes；
(3) 90 DEG C are warming up to, is stirred 1 hour, cooling, suction filtration is washed with a small amount, dries, obtains 2,7- dichloro fluorenes
160g。
Embodiment 2：
The preparation method of one kind 2,7- dichloro fluorenes, comprises the following steps：
(1) 200g fluorenes, 500ml glacial acetic acids, 0.2g anhydrous ferric trichlorides are added in reactor, temperature is increased to 20 DEG C；
(2) appropriate chlorine is passed through, sampling detection, when HPLC detects chlorine fluorenes purity≤5% of reaction intermediate one, stops logical
Chlorine, continues to stir 10 minutes；
(3) 90 DEG C are warming up to, is stirred 1 hour, cooling, suction filtration is washed with a small amount, dries, obtains 2,7- dichloro fluorenes
170g。
Embodiment 3：
The preparation method of one kind 2,7- dichloro fluorenes, comprises the following steps：
(1) 200g fluorenes, 600ml glacial acetic acids, 0.2g anhydrous ferric trichlorides are added in reactor, temperature is increased to 20 DEG C；
(2) appropriate chlorine is passed through, sampling detection, when HPLC detects chlorine fluorenes purity≤5% of reaction intermediate one, stops logical
Chlorine, continues to stir 10 minutes；
(3) 90 DEG C are warming up to, is stirred 1 hour, cooling, suction filtration is washed with a small amount, dries, obtains 2,7- dichloro fluorenes
150g。
Claims (2)
1. the preparation method of one kind 2,7- dichloro fluorenes, comprises the following steps：
(1) 200g fluorenes, 400-600ml glacial acetic acids, 0.2g anhydrous ferric trichlorides are added in reactor, temperature is increased to 20 DEG C；
(2) appropriate chlorine is passed through, sampling detection, when HPLC detects chlorine fluorenes purity≤5% of reaction intermediate one, stops logical chlorine, after
Continuous stirring 10 minutes；
(3) 90 DEG C are warming up to, is stirred 1 hour, cooling, suction filtration is washed with a small amount, dries, obtains 2,7- dichloro fluorenes.
2. the preparation method of a kind of 2,7- dichloros fluorenes according to claim 1, it is characterised in that comprise the following steps：
(1) 200g fluorenes, 500ml glacial acetic acids, 0.2g anhydrous ferric trichlorides are added in reactor, temperature is increased to 20 DEG C；
(2) appropriate chlorine is passed through, sampling detection, when HPLC detects chlorine fluorenes purity≤5% of reaction intermediate one, stops logical chlorine, after
Continuous stirring 10 minutes；
(3) 90 DEG C are warming up to, is stirred 1 hour, cooling, suction filtration is washed with a small amount, dries, obtains 2,7- dichloro fluorenes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710530237.4A CN107285990A (en) | 2017-06-24 | 2017-06-24 | A kind of preparation method of 2,7 dichloro fluorenes |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710530237.4A CN107285990A (en) | 2017-06-24 | 2017-06-24 | A kind of preparation method of 2,7 dichloro fluorenes |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107285990A true CN107285990A (en) | 2017-10-24 |
Family
ID=60099935
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710530237.4A Pending CN107285990A (en) | 2017-06-24 | 2017-06-24 | A kind of preparation method of 2,7 dichloro fluorenes |
Country Status (1)
| Country | Link |
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| CN (1) | CN107285990A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108586189A (en) * | 2018-06-04 | 2018-09-28 | 绍兴文理学院 | A kind of recovery and treatment method of 2,7- dichloros fluorenes reaction mother liquor |
-
2017
- 2017-06-24 CN CN201710530237.4A patent/CN107285990A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108586189A (en) * | 2018-06-04 | 2018-09-28 | 绍兴文理学院 | A kind of recovery and treatment method of 2,7- dichloros fluorenes reaction mother liquor |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20171024 |
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| WD01 | Invention patent application deemed withdrawn after publication |