CN106831571A - A kind of nivaquin production technology - Google Patents
A kind of nivaquin production technology Download PDFInfo
- Publication number
- CN106831571A CN106831571A CN201710075341.9A CN201710075341A CN106831571A CN 106831571 A CN106831571 A CN 106831571A CN 201710075341 A CN201710075341 A CN 201710075341A CN 106831571 A CN106831571 A CN 106831571A
- Authority
- CN
- China
- Prior art keywords
- alkali
- pot
- salt
- toluene
- condensation
- 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.)
- Pending
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D215/00—Heterocyclic compounds containing quinoline or hydrogenated quinoline ring systems
- C07D215/02—Heterocyclic compounds containing quinoline or hydrogenated quinoline ring systems having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen atoms or carbon atoms directly attached to the ring nitrogen atom
- C07D215/16—Heterocyclic compounds containing quinoline or hydrogenated quinoline ring systems having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen atoms or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D215/38—Nitrogen atoms
- C07D215/42—Nitrogen atoms attached in position 4
- C07D215/46—Nitrogen atoms attached in position 4 with hydrocarbon radicals, substituted by nitrogen atoms, attached to said nitrogen atoms
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Dichloroquinoline is a kind of important chemical products, is widely used in daily life.The present invention provides a kind of nivaquin production technology, including：1. alkali condensation；2. into salt；3. refine.
Description
Technical field
The present invention relates to chemical production field, especially nivaquin production field.
Background technology
Dichloroquinoline is a kind of important chemical products, is widely used in daily life.
The content of the invention
The present invention provides a kind of nivaquin production technology, including：1. alkali condensation；2. into salt；3. refine.Detailed process
It is as follows：
1. alkali condensation：By in dichloroquinoline input alkali condensation reaction pot, the phenol of melting in advance, crawl stirring, nothing are pumped into
Stirring is opened after exception, side chain is added, condensation reaction is started after uniform temperature is to slowly warm up to after adding, temperature is controlled in reaction
Degree.Liquid caustic soda and water are added in alkalization pot, completely reacted condensation product is gone out and is stirred heat up alkalization, cooling of having alkalized to alkalization pot
Extracted by several times with toluene afterwards free alkali to toluene layer it is colourless.Buck is taken out in being put into storage tank.Alkali toluene liquid merges
In washing in pot, washed by several times with drinking water, a point most water layer is stood after washing.Alkali toluene liquid is filtered to transfer pot,
Then concentration pan is sucked, toluene is fallen in vacuum distillation, is to stop extremely without distillate.Sampling, discharging to measuring tank heat preservation for standby use.
2. into salt：The ethanol that will be measured is squeezed into salt pan, and alkali in alkali measuring tank is pressed into into salt under agitation
In pot, the phosphoric acid of amount of calculation is then pressed into salt pan, controls kettle temperature, stirring to crystallization is separated out.Crystal after analysis, is sampled entirely
After survey pH values are qualified, progressively start decrease temperature crystalline, centrifugation, washing, lower post is handed over after obtaining the metering of chloroquine diphosphate crude product.It is female
Liquid pump is squeezed into thick female recovery, and ethanol is reclaimed in air-distillation, and after about 2-3 batches, the interior material of vacuum distillation pot goes out in thick
Material, waste residue is abandoned.
3. refine：Chloroquine diphosphate crude product is put into dissolving pan, purified water is added, stirring heats up.Treat that crude product is completely dissolved
Afterwards, surface oil reservoir is removed.The qualified rear suction Decolouring pot of pH values is determined, addition pure water soaks to obtain activated carbon insulation into pasty state
Stirring is decolourized.Press filtration after the completion of decolouring, destainer is depressed into transfer tank.Ethanol crystallisation by cooling is added after measurement, body to be crystallized is complete
After analysis through centrifugation, washing, drying, pulverize and sieve.
Brief description of the drawings：
Fig. 1 is reaction equation.
Claims (3)
1. the present invention provides a kind of nivaquin production technology, including：1. alkali condensation；2. into salt；3. refine.
2. the alkali condensation of claim 1 description is pumped into the benzene of melting in advance by dichloroquinoline input alkali condensation reaction pot
Phenol, crawl stirring, it is without exception after open stirring, add side chain, start condensation reaction after uniform temperature is to slowly warm up to after adding,
Temperature is controlled in reaction；Liquid caustic soda and water are added in alkalization pot, completely reacted condensation product is gone out and is stirred intensification alkali to alkalization pot
Change, after cooling of alkalize with toluene by several times extract dissociate alkali to toluene layer it is colourless；Buck is taken out in being put into storage tank；Salt
Base toluene liquid is incorporated in be washed in pot, is washed by several times with drinking water, and a point most water layer is stood after washing；Alkali toluene liquid is through filter mistake
Then filter sucks concentration pan to transfer pot, and toluene is fallen in vacuum distillation, is to stop extremely without distillate；Sampling, discharging to measuring tank insulation
It is stand-by.
3. the ethanol that will be measured into salt of claim 1 description is squeezed into salt pan, under agitation by alkali measuring tank inner salt
Base is pressed into salt pan, and the phosphoric acid of amount of calculation then is pressed into into salt pan, controls kettle temperature, and stirring to crystallization is separated out；Crystal
After full analysis, after sampling survey pH values are qualified, progressively start decrease temperature crystalline, centrifugation, washing, after obtaining the metering of chloroquine diphosphate crude product
Hand over lower post；Mother liquor pump is squeezed into thick female recovery, and ethanol is reclaimed in air-distillation, after about 2-3 batches, the interior material of vacuum distillation pot
In thick, discharging, waste residue discarding.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710075341.9A CN106831571A (en) | 2017-02-13 | 2017-02-13 | A kind of nivaquin production technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710075341.9A CN106831571A (en) | 2017-02-13 | 2017-02-13 | A kind of nivaquin production technology |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106831571A true CN106831571A (en) | 2017-06-13 |
Family
ID=59127948
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710075341.9A Pending CN106831571A (en) | 2017-02-13 | 2017-02-13 | A kind of nivaquin production technology |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106831571A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111662229A (en) * | 2020-07-08 | 2020-09-15 | 精华制药集团南通有限公司 | Preparation process of chloroquine phosphate |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017004454A1 (en) * | 2015-06-30 | 2017-01-05 | Eiger Group International, Inc. | Use of chloroquine and clemizole compounds for treatment of inflammatory and cancerous conditions |
-
2017
- 2017-02-13 CN CN201710075341.9A patent/CN106831571A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017004454A1 (en) * | 2015-06-30 | 2017-01-05 | Eiger Group International, Inc. | Use of chloroquine and clemizole compounds for treatment of inflammatory and cancerous conditions |
Non-Patent Citations (1)
| Title |
|---|
| 罗彦凤等: "硫酸氯喹的精制工艺改进", 《重庆大学学报（自然科学版）》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111662229A (en) * | 2020-07-08 | 2020-09-15 | 精华制药集团南通有限公司 | Preparation process of chloroquine phosphate |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170613 |