CN106916120A - A kind of synthetic method of high-purity docetaxel - Google Patents
A kind of synthetic method of high-purity docetaxel Download PDFInfo
- Publication number
- CN106916120A CN106916120A CN201510991605.6A CN201510991605A CN106916120A CN 106916120 A CN106916120 A CN 106916120A CN 201510991605 A CN201510991605 A CN 201510991605A CN 106916120 A CN106916120 A CN 106916120A
- Authority
- CN
- China
- Prior art keywords
- docetaxel
- acetic acid
- glacial acetic
- purity
- synthetic method
- 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
- C07D—HETEROCYCLIC COMPOUNDS
- C07D305/00—Heterocyclic compounds containing four-membered rings having one oxygen atom as the only ring hetero atoms
- C07D305/14—Heterocyclic compounds containing four-membered rings having one oxygen atom as the only ring hetero atoms condensed with carbocyclic rings or ring systems
Abstract
The invention discloses a kind of synthetic method of high-purity docetaxel, comprise the following steps：1) docetaxel intermediate is dissolved in glacial acetic acid, adds first alcohol and water, the docetaxel intermediate, the mass volume ratio of glacial acetic acid are 1:5~15, the mass volume ratio of first alcohol and water is 1：10~20, the glacial acetic acid is 2 with the mass volume ratio of methyl alcohol:1~1.5；2) 1 to 2 hours of stirring reaction；3) zinc powder, 2 to 3 hours of stirring reaction are added；4) filter, step 3 is obtained into product and is filtered, obtain the solid for separating out；5) solid that step 4 is obtained is purified, is obtained docetaxel.The synthetic method synthesis step of high-purity docetaxel of the invention is simple, and production efficiency is high, and the product purity of acquisition is high.
Description
Technical field
The present invention relates to docetaxel field, a kind of conjunction of high-purity docetaxel is specifically related to
Into method.
Background technology
Docetaxel is a kind of conventional medicine, and its chemical name is 2aR- (2a α, 4 β, 4a β, 6
β, 9 α, (α R ', β S '), 11 α, 12 α, 12a α, 12b α)-β -1,1- dimethylethoxies
Base carbonylamino-alpha-carbonyl benzenpropanoic acid 12b- acetyl oxygen -12- benzoxy -2a, 3,4,4a, 5,6,9,10,
Dihydro -4,6,11- trihydroxies -4a, the 8,13,13- tetramethyl -5- oxos -7,11- of 11,12,12a, 12b- ten is sub-
Methyl isophthalic acid H- ring last of the ten Heavenly stems pentaenes and 3,4 benzo 1,2-b oxa- fourth ring -9- base esters.Existing docetaxel
The docetaxel purity that synthetic method is obtained is relatively low, and contains more impurity.
The content of the invention
(1) technical problem to be solved
In view of the shortcomings of the prior art, the present invention provides a kind of conjunction of high-purity docetaxel
Into method.
(2) technical scheme
To reach above-mentioned purpose, the invention provides a kind of synthesis side of high-purity docetaxel
Method, comprises the following steps：
1) docetaxel intermediate is dissolved in glacial acetic acid, adds first alcohol and water, it is described many
Xi Tasai intermediates, the mass volume ratio of glacial acetic acid are 1:5~15, the quality volume of first alcohol and water
Than being 1：10~20, the glacial acetic acid is 2 with the mass volume ratio of methyl alcohol:1~1.5；
2) 1 to 2 hours of stirring reaction；
3) zinc powder, 2 to 3 hours of stirring reaction are added；
4) filter, step 3 is obtained into product and is filtered, obtain the docetaxel for separating out thick
Product；
5) docetaxel crude product ethyl acetate is dissolved；
6) lower addition petroleum ether, the volume of ethyl acetate in the petroleum ether and step 5 are stirred
Than being 1:1~4；
7) stirring separates out complete for 5~8 hours to solid.
Further, docetaxel intermediate, the mass volume ratio of glacial acetic acid in the step 1
It is 1:6.
Further, the reaction temperature of the step 2 and step 3 is 40 ° to 60 °.
(3) beneficial effect
The synthetic method synthesis step of high-purity docetaxel of the present invention is simple, and production efficiency is high,
The product purity of acquisition is high.
Specific embodiment
With reference to embodiment, specific embodiment of the invention is described in further detail.
Following examples are used to illustrate the present invention, but are not limited to the scope of the present invention.
A kind of synthetic method of high-purity docetaxel of the invention, comprises the following steps：
1) docetaxel intermediate is dissolved in glacial acetic acid, adds first alcohol and water, it is described many
Xi Tasai intermediates, the mass volume ratio of glacial acetic acid are 1:5~15, the quality volume of first alcohol and water
Than being 1：10~20, the glacial acetic acid is 2 with the mass volume ratio of methyl alcohol:1~1.5；
2) 1 to 2 hours of stirring reaction；
3) zinc powder, 2 to 3 hours of stirring reaction are added；
4) filter, step 3 is obtained into product and is filtered, obtain the docetaxel for separating out thick
Product；
5) docetaxel crude product ethyl acetate is dissolved；
6) lower addition petroleum ether, the volume of ethyl acetate in the petroleum ether and step 5 are stirred
Than being 1:1~4；
7) stirring separates out complete for 5~8 hours to solid.
In the present embodiment, docetaxel intermediate, the quality of glacial acetic acid in the step 1
Volume ratio is 1:6.
In the present embodiment, the reaction temperature of the step 2 and step 3 is 40 ° to 60 °.
Beneficial effects of the present invention：Synthesis step is simple, and production efficiency is high, and the product of acquisition is pure
Degree is high.
The above is only the preferred embodiment of the present invention, it is noted that led for this technology
For the those of ordinary skill in domain, on the premise of the technology of the present invention principle is not departed from, can be with
Some improvements and modifications are made, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (3)
1. a kind of synthetic method of high-purity docetaxel, it is characterised in that including following step
Suddenly：
1) docetaxel intermediate is dissolved in glacial acetic acid, adds first alcohol and water, it is described many
Xi Tasai intermediates, the mass volume ratio of glacial acetic acid are 1:5~15, the quality volume of first alcohol and water
Than being 1：10~20, the glacial acetic acid is 2 with the mass volume ratio of methyl alcohol:1~1.5；
2) 1 to 2 hours of stirring reaction；
3) zinc powder, 2 to 3 hours of stirring reaction are added；
4) filter, step 3 is obtained into product and is filtered, obtain the docetaxel for separating out thick
Product；
5) docetaxel crude product ethyl acetate is dissolved；
6) lower addition petroleum ether, the volume of ethyl acetate in the petroleum ether and step 5 are stirred
Than being 1:1~4；
7) stirring separates out complete for 5~8 hours to solid.
2. the synthetic method of high-purity docetaxel as claimed in claim 1, its feature exists
In docetaxel intermediate, the mass volume ratio of glacial acetic acid are 1 in the step 1:6.
3. the synthetic method of high-purity docetaxel as claimed in claim 1, its feature exists
In the reaction temperature of the step 2 and step 3 is 40 ° to 60 °.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510991605.6A CN106916120A (en) | 2015-12-25 | 2015-12-25 | A kind of synthetic method of high-purity docetaxel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510991605.6A CN106916120A (en) | 2015-12-25 | 2015-12-25 | A kind of synthetic method of high-purity docetaxel |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106916120A true CN106916120A (en) | 2017-07-04 |
Family
ID=59459474
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510991605.6A Pending CN106916120A (en) | 2015-12-25 | 2015-12-25 | A kind of synthetic method of high-purity docetaxel |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106916120A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109836401A (en) * | 2017-11-28 | 2019-06-04 | 正大天晴药业集团股份有限公司 | A kind of purification process of docetaxel |
-
2015
- 2015-12-25 CN CN201510991605.6A patent/CN106916120A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109836401A (en) * | 2017-11-28 | 2019-06-04 | 正大天晴药业集团股份有限公司 | A kind of purification process of docetaxel |
| CN109836401B (en) * | 2017-11-28 | 2023-02-14 | 正大天晴药业集团股份有限公司 | Method for purifying docetaxel |
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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: 20170704 |