CN106916126A - A kind of process for purification of docetaxel - Google Patents
A kind of process for purification of docetaxel Download PDFInfo
- Publication number
- CN106916126A CN106916126A CN201510997156.6A CN201510997156A CN106916126A CN 106916126 A CN106916126 A CN 106916126A CN 201510997156 A CN201510997156 A CN 201510997156A CN 106916126 A CN106916126 A CN 106916126A
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- CN
- China
- Prior art keywords
- docetaxel
- volume ratio
- acetic acid
- purification
- alcohol
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- 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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- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of process for purification of 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) carry out refining for the first time, 6) refine for the second time.The process for purification synthesis step of 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 refined side of docetaxel is specifically related to
Method.
Background technology
Docetaxel, its chemical name be 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- dimethylethoxy-carbonyl amino-α -
Carbonyl benzenpropanoic acid 12b- acetyl oxygen -12- benzoxies -2a, 3,4,4a, 5,6,9,10,11,12,12a, 12b-
Ten dihydro -4,6,11- trihydroxies -4a, the 8,13,13- tetramethyl -5- oxo -7,11- methylene -1H- ring last of the ten Heavenly stems
Pentaene and 3,4 benzo 1,2-b oxa- fourth ring -9- base esters.It is a kind of conventional medicine, it is existing many
Xi Tasai synthetic method complex steps, production efficiency is low.
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 refined side of docetaxel
Method.
(2) technical scheme
To reach above-mentioned purpose, the invention provides a kind of process for purification of docetaxel, bag
Include following steps：
1) docetaxel intermediate is dissolved in methyl alcohol, the docetaxel intermediate, methyl alcohol
Mass volume ratio be 1:10, add the quality of acetic acid, the docetaxel intermediate and acetic acid
Volume ratio is 1:3.5；
2) half hour of stirring reaction；
3) zinc powder, 1 hour of stirring reaction are added；
4) filter, step 3 is obtained into solidliquid mixture and is filtered, obtain the west more for separating out
He matches crude product；
5) it is refined for the first time：Docetaxel crude product is dissolved with ethyl acetate, petroleum ether is added,
Crystallization, filtering, dry docetaxel first time highly finished product, the ethyl acetate and petroleum ether
Volume ratio be 1: 10~100；
6) refine for second：With first time highly finished product in lower alcohol dissolving step 5, add
Water, crystallization, filtering, dry second highly finished product of docetaxel, the lower alcohol and water
Volume ratio is 1: 10~100, and the lower alcohol is any one in ethanol, methyl alcohol, propyl alcohol.
Further, docetaxel intermediate, the mass volume ratio of glacial acetic acid in the step 1
It is 1:8.
Further, the reaction temperature of the step 2 and step 3 is 20 ° to 60 °.
(3) beneficial effect
The process for purification synthesis step of docetaxel of the present invention is simple, and production efficiency is high, acquisition
Product purity 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 process for purification of docetaxel of the invention, comprises the following steps：
1) docetaxel intermediate is dissolved in methyl alcohol, the docetaxel intermediate, methyl alcohol
Mass volume ratio be 1:10, add the quality of acetic acid, the docetaxel intermediate and acetic acid
Volume ratio is 1:3.5；
2) half hour of stirring reaction；
3) zinc powder, 1 hour of stirring reaction are added；
4) filter, step 3 is obtained into solidliquid mixture and is filtered, obtain the west more for separating out
He matches crude product；
5) it is refined for the first time：Docetaxel crude product is dissolved with ethyl acetate, petroleum ether is added,
Crystallization, filtering, dry docetaxel first time highly finished product, the ethyl acetate and petroleum ether
Volume ratio be 1: 10~100；
6) refine for second：With first time highly finished product in lower alcohol dissolving step 5, add
Water, crystallization, filtering, dry second highly finished product of docetaxel, the lower alcohol and water
Volume ratio is 1: 10~100, and the lower alcohol is any one in ethanol, methyl alcohol, propyl alcohol.
In the present embodiment, docetaxel intermediate, the quality of glacial acetic acid in the step 1
Volume ratio is 1:8.
In the present embodiment, the reaction temperature of the step 2 and step 3 is 20 ° 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 process for purification of docetaxel, it is characterised in that comprise the following steps：
1) docetaxel intermediate is dissolved in methyl alcohol, the docetaxel intermediate, methyl alcohol
Mass volume ratio be 1:10, add the quality of acetic acid, the docetaxel intermediate and acetic acid
Volume ratio is 1:3.5；
2) half hour of stirring reaction；
3) zinc powder, 1 hour of stirring reaction are added；
4) filter, step 3 is obtained into solidliquid mixture and is filtered, obtain the west more for separating out
He matches crude product；
5) it is refined for the first time：Docetaxel crude product is dissolved with ethyl acetate, petroleum ether is added,
Crystallization, filtering, dry docetaxel first time highly finished product, the ethyl acetate and petroleum ether
Volume ratio be 1: 10~100；
6) refine for second：With first time highly finished product in lower alcohol dissolving step 5, add
Water, crystallization, filtering, dry second highly finished product of docetaxel, the lower alcohol and water
Volume ratio is 1: 10~100, and the lower alcohol is any one in ethanol, methyl alcohol, propyl alcohol.
2. the process for purification of docetaxel as claimed in claim 1, it is characterised in that institute
State docetaxel intermediate in step 1, the mass volume ratio of glacial acetic acid is 1:8.
3. the process for purification of docetaxel as claimed in claim 1, it is characterised in that institute
The reaction temperature for stating step 2 and step 3 is 20 ° to 60 °.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510997156.6A CN106916126A (en) | 2015-12-25 | 2015-12-25 | A kind of process for purification of docetaxel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510997156.6A CN106916126A (en) | 2015-12-25 | 2015-12-25 | A kind of process for purification of docetaxel |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106916126A true CN106916126A (en) | 2017-07-04 |
Family
ID=59455695
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510997156.6A Pending CN106916126A (en) | 2015-12-25 | 2015-12-25 | A kind of process for purification of docetaxel |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106916126A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110305080A (en) * | 2019-08-12 | 2019-10-08 | 新乡双鹭药业有限公司 | A kind of purification process of docetaxel |
-
2015
- 2015-12-25 CN CN201510997156.6A patent/CN106916126A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110305080A (en) * | 2019-08-12 | 2019-10-08 | 新乡双鹭药业有限公司 | A kind of purification process of docetaxel |
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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: 20170704 |
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| WD01 | Invention patent application deemed withdrawn after publication |