CN104610194B - The method that fenazil oxalates is reclaimed in the mother liquor of hydrochloric acid - Google Patents
The method that fenazil oxalates is reclaimed in the mother liquor of hydrochloric acid Download PDFInfo
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- CN104610194B CN104610194B CN201410595170.9A CN201410595170A CN104610194B CN 104610194 B CN104610194 B CN 104610194B CN 201410595170 A CN201410595170 A CN 201410595170A CN 104610194 B CN104610194 B CN 104610194B
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- solid
- oxalates
- fenazil
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- added dropwise
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D279/00—Heterocyclic compounds containing six-membered rings having one nitrogen atom and one sulfur atom as the only ring hetero atoms
- C07D279/10—1,4-Thiazines; Hydrogenated 1,4-thiazines
- C07D279/14—1,4-Thiazines; Hydrogenated 1,4-thiazines condensed with carbocyclic rings or ring systems
- C07D279/18—[b, e]-condensed with two six-membered rings
- C07D279/22—[b, e]-condensed with two six-membered rings with carbon atoms directly attached to the ring nitrogen atom
- C07D279/24—[b, e]-condensed with two six-membered rings with carbon atoms directly attached to the ring nitrogen atom with hydrocarbon radicals, substituted by amino radicals, attached to the ring nitrogen atom
- C07D279/26—[b, e]-condensed with two six-membered rings with carbon atoms directly attached to the ring nitrogen atom with hydrocarbon radicals, substituted by amino radicals, attached to the ring nitrogen atom without other substituents attached to the ring system
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of extracting method of promethazine hydrochloride in mother liquor, a kind of method for being related specifically to reclaim fenazil oxalates in mother liquor of hydrochloric acid.It is characterized in that：By promethazine hydrochloride crystalline mother solution, it is evaporated, obtains solid, obtained solid is dissolved with water, drip off 50 degree or so and be incubated 1 hour, be incubated again plus toluene extraction, extract and has taken toluene layer, addition 0.05 times of weight than activated carbon decolorizing, filtering, toluene liquid after filtering is evaporated under reduced pressure, extremely without distillate, then methanol is added into concentrate（Four times of weight ratios of solid）, the oxalic acid methanol solution that 2 times of moles are wherein added dropwise is rethought, is added dropwise, is flowed back 2 hours, rear crystallisation by cooling to temperature refilters washing and drying and obtain fenazil oxalates to 10 to 15 degree.
Description
Technical field
The present invention relates to a kind of extracting method of promethazine hydrochloride in mother liquor, is related specifically in a kind of mother liquor of hydrochloric acid
The method for reclaiming fenazil oxalates.
Background technology
The brief introduction of promethazine hydrochloride：
Promethazine hydrochloride (English：Promethazine, also known as Diprazine Hydrochloride (Promethazine
Hydrochloride) or phenergan (Phenergan)) be a kind of common cough suppressing medicine, be a kind of antithistamine, can be competing
Striving property blocking histamine H1 acceptors, to the telangiectasis caused by antihistamine, and reduce its permeability.Therefore, it is possible to calm down because
For tracheae it is stimulated caused by cough.
Can competitive blocking histamine Hl acceptors and produce antihistamine effect, can to the telangiectasis caused by antihistamine,
Its permeability is reduced, alleviates panting caused by bronchial smooth muscle shrinks, reduces environmental pollution, turn waste into wealth, improve raw material
Reuse ratio.
In the mother liquor of the final refining of promethazine hydrochloride (between the amount of promethazine hydrochloride is about 5%~10% in mother liquor)
In, small part promethazine hydrochloride and partial impurities that sub-fraction does not separate out be present, be dissolved in using acetone as solvent
In mother liquor, this, the purpose of method is that the promethazine hydrochloride for abandoning this part is therefrom taken out, and is reached by processing
Standard, taken out with the identity of oxalates, then promethazine hydrochloride is made.
The content of the invention
The technical problems to be solved by the invention are：Reduce environmental pollution, turn waste into wealth, improve the reuse ratio of raw material.
To complete foregoing invention purpose, the present invention is that so this is existing：By promethazine hydrochloride crystalline mother solution, it is evaporated, must consolidates
Body (to weigh, solid is promethazine hydrochloride and its impurity), obtained solid is dissolved into (water of four times of amounts of solid) with water,
Liquid caustic soda (liquid caustic soda is 30% or so liquid caustic soda, and dosage is 1.1 times of moles of solid) is added dropwise again, it is small to drip off 50 degree or so insulations 1
When, it has been incubated again plus toluene extracts (dosage asks 2 times of weight ratios of solid), has extracted and taken toluene layer, added 0.05 times of weight ratio
Activated carbon decolorizing (50 degree decolourize 15 minutes), filtering, the toluene liquid after filtering is evaporated under reduced pressure, to without distillate (temperature control
System is at 60 degree), then methanol (four times of weight ratios of solid) is added into concentrate, rethink the oxalic acid that 2 times of moles are wherein added dropwise
(oxalic acid methanol ratio is 1 to methanol solution：1), it is added dropwise, flows back 2 hours, rear crystallisation by cooling to temperature to 10 to 15 is spent, then
Filtration washing dries to obtain fenazil oxalates.
Brief description of the drawings
Fig. 1 is technological reaction flow chart.
Described weight ratio in figure, and mol ratio, the solid (promethazine hydrochloride and a small amount of after crystalline mother solution is evaporated
Impurity) it is control.
Embodiment
Embodiment 1：
3kg promethazine hydrochloride mother liquors are evaporated to obtain 175g promethazine hydrochloride crude solids, in 1000ml four-hole boiling flask
Middle addition 100g solids, add 400g water, stirring and dissolving, then 45.7g30% liquid caustic soda are added dropwise (amount of alkali is solid in liquid caustic soda
The mol ratio that 1.1 times of thing).Be added dropwise 50 degree insulation 1h, insulation finish plus 200g toluene extraction, be layered, toluene layer, then to
5g activated carbons are added in toluene liquid, 50 degree of insulations are decolourized, decolourize to finish, filter, the toluene liquid filtered is subtracted at 60 degree for 15 minutes
Pressure distillation adds 400g methanol, toluene liquid concentrate is dissolved, add 112g oxalic acid methanol solution (grass to without distillate
The weight ratio of sour methanol is 1：1), back flow reaction 2 hours, then 10~15 degree are cooled to, product fenazil oxalates is separated out, after
Filter, washing and drying obtain fenazil oxalates 93.2g, yield 79.9%.
Claims (1)
1. the method for fenazil oxalates is reclaimed in a kind of crystalline mother solution from promethazine hydrochloride, it is characterised in that：By hydrochloric acid isopropyl
Piperazine crystalline mother solution, is evaporated, and obtains solid, and obtained solid is dissolved with water, then liquid caustic soda is added dropwise, and is dripped off 50 degree and is incubated 1 hour, insulation
It is complete again plus toluene extraction, extract and has taken toluene layer, add 0.05 times of weight than activated carbon decolorizing, filter, by the first after filtering
Benzene liquid is evaporated under reduced pressure, and extremely without distillate, then methanol is added into concentrate, and the weight of methanol is four times of weight of solid, then to
The oxalic acid methanol solution of 2 times of moles is wherein added dropwise, is added dropwise, flows back 2 hours, rear crystallisation by cooling to temperature to 10 to 15
Degree, refilters washing and drying and obtains fenazil oxalates；Solid is promethazine hydrochloride and its impurity；The dosage of described water is solid
Four times of the dosage of body；Described liquid caustic soda is 30% liquid caustic soda, and dosage is 1.1 times of moles of solid；By the toluene after filtering
Liquid is evaporated under reduced pressure, extremely without distillate temperature control at 60 degree；Described oxalic acid methanol ratio is 1：1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410595170.9A CN104610194B (en) | 2014-10-30 | 2014-10-30 | The method that fenazil oxalates is reclaimed in the mother liquor of hydrochloric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410595170.9A CN104610194B (en) | 2014-10-30 | 2014-10-30 | The method that fenazil oxalates is reclaimed in the mother liquor of hydrochloric acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104610194A CN104610194A (en) | 2015-05-13 |
| CN104610194B true CN104610194B (en) | 2017-12-26 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410595170.9A Active CN104610194B (en) | 2014-10-30 | 2014-10-30 | The method that fenazil oxalates is reclaimed in the mother liquor of hydrochloric acid |
Country Status (1)
| Country | Link |
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| CN (1) | CN104610194B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113292513B (en) * | 2021-05-25 | 2022-03-25 | 常州康普药业有限公司 | Preparation method of high-purity promethazine hydrochloride |
| CN115974813A (en) * | 2022-12-20 | 2023-04-18 | 云鹏医药集团有限公司 | Synthetic method of high-purity promethazine hydrochloride |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2607773A (en) * | 1952-08-19 | Processes for preparing phenthi- | ||
| US2526118A (en) * | 1950-10-17 | Paul chabpentier | ||
| DE1181223B (en) * | 1962-07-14 | 1964-11-12 | Dresden Arzneimittel | Process for the industrial production of phenthiazine bases |
| CN102617608A (en) * | 2012-03-09 | 2012-08-01 | 常州大学 | Methods for synthesizing and separating isothipendyl serving as antihistamine medicine |
| CN102924484A (en) * | 2012-11-13 | 2013-02-13 | 常州大学 | Industrial production method of isothipendyl technical material |
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2014
- 2014-10-30 CN CN201410595170.9A patent/CN104610194B/en active Active
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| Publication number | Publication date |
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| CN104610194A (en) | 2015-05-13 |
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| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 226532 No. 10, Yuejiang Road, Changjiang town (Rugao port area), Rugao City, Nantong City, Jiangsu Province Patentee after: Jiangsu Baozhong Baoda Pharmaceutical Co.,Ltd. Address before: 226532 No. 10, Yuejiang Road, Changjiang town (Rugao port area), Rugao City, Nantong City, Jiangsu Province Patentee before: JIANGSU BAOZONG & BAODA PHARMACHEM Co.,Ltd. |