CN104402708A - Production method for sodium camphorate - Google Patents
Production method for sodium camphorate Download PDFInfo
- Publication number
- CN104402708A CN104402708A CN201410732813.XA CN201410732813A CN104402708A CN 104402708 A CN104402708 A CN 104402708A CN 201410732813 A CN201410732813 A CN 201410732813A CN 104402708 A CN104402708 A CN 104402708A
- Authority
- CN
- China
- Prior art keywords
- sodium
- production method
- camphorsulfonate
- camphorsulfonic acid
- dextrocamphoric
- 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
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/32—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of salts of sulfonic acids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/42—Separation; Purification; Stabilisation; Use of additives
- C07C303/44—Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2602/00—Systems containing two condensed rings
- C07C2602/36—Systems containing two condensed rings the rings having more than two atoms in common
- C07C2602/42—Systems containing two condensed rings the rings having more than two atoms in common the bicyclo ring system containing seven carbon atoms
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention relates to a production method for preparing a medicine using sodium camphorate as a raw material by a spray drying method. The method comprises the following steps of dissolving camphorsulfonic acid which serves as a raw material in water, performing decolorization by using activated carbon, and regulating the pH value to obtain clear feed liquor by using sodium bicarbonate; performing spray-drying on the feed liquor to obtain a medicine product using sodium camphorate as the raw material. According to the production method, the problem of difficulty in drying during the preparation of sodium camphorate through a conventional method is solved, the industrial production efficiency is greatly improved, and the prepared product has the advantages of high content, high yield, good color and the like.
Description
Technical field
The invention belongs to medicinal chemistry art, be specifically related to a kind of production method of central stimulant, particularly a kind of production method of dextrocamphoric acid sodium.
Background technology
Sodium camphorsulfonate is central nervous system stimulants, has the effect of excited respiratory centre and vasomotor center, also has cardiotonic, is mainly used in the acute disorder of breathing that the poisoning and pneumonia of curative etc. causes and circulation, resists the poisoning etc. of nervus centralis.Sodium camphorsulfonate is crystallization or the crystalline powder of white, easily molten in water or hot ethanol.Sodium camphorsulfonate is low because of its good effect, price, is widely used in veterinary drug.
In prior art, the synthesis of sodium camphorsulfonate is by camphorsulfonic acid and deionized water 1: 0.8 weight proportion, camphorsulfonic acid is dissolved in deionized water, add the sodium bicarbonate stirring reaction of about 0.35 times, and regulate reacting liquid pH value to be 7 with sodium bicarbonate, then add 0.01 times activated carbon decolorizing filter, filtrate reduced in volume to starching thick crystalloid, rejection filter while hot, drying, obtains sodium camphorsulfonate.
The production method of prior art obtains sodium camphorsulfonate, and decolorizing effect is bad, and color is somewhat yellow, in addition difficult oven dry, and drying time is longer, thus have impact on sodium camphorsulfonate production efficiency and quality product.
Therefore, in the urgent need to a kind of good decolorizing effect, easily dry method produces sodium camphorsulfonate.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide one to be easy to drying, yield is high, content is high, the preparation method of the dextrocamphoric acid sodium that color is good-looking.
For achieving the above object, the concrete technical scheme that the present invention adopts is: a kind of production method of dextrocamphoric acid sodium, it comprises the following steps: added by camphorsulfonic acid in purified water, 60 ~ 80 DEG C are warming up under stirring, dissolve completely in backward solution and add gac, leave standstill decolouring 30 ~ 60min, then filtered while hot, filtrate is transferred in the reactor of a cleaning, be heated to 80 ~ 95 DEG C, then the pH value adding manganese hydrogen sodium regulating solution is 6.0-7.0, obtain sodium camphorsulfonate feed liquid, sodium camphorsulfonate feed liquid is carried out spraying dry, sodium camphorsulfonate product.
Described camphorsulfonic acid and the weight ratio of purified water are 1: 0.5-5.
The consumption of described gac is 2 ~ 5% of camphorsulfonic acid quality.
Described sodium bicarbonate quality is the 0.38-0.55 of camphorsulfonic acid quality.
Described spray-dired condition is inlet temperature 130-150 DEG C, and atomization frequency 8000-10000rpm, air outlet temperature is 60-85 DEG C, and the flow velocity of feed control peristaltic pump is 40-60rpm.
Compared with prior art, the present invention has following beneficial effect:
The method that the present invention produces sodium camphorsulfonate bulk drug makes product content reach more than 99%; And the product yield of gained significantly improves, yield is up to more than 98%.The invention solves sodium camphorsulfonate in prior art production process and dry difficult problem, obtained product has the advantages such as content is high, yield is high, color is good.This production method makes the production efficiency of sodium camphorsulfonate bulk drug significantly improve, and can meet the needs that enterprise produces very well.
Embodiment
Below in conjunction with embodiment, the present invention is elaborated, instead of limit protection scope of the present invention.
Embodiment 1
By 500kg camphorsulfonic acid, 1000kg pure water adds in reactor, 60 DEG C are warming up under stirring, dissolve completely in backward solution and add 10kg gac, leave standstill decolouring 30 ~ 60min, then filtered while hot, filtrate is transferred in the reactor of a cleaning, be heated to 80 DEG C, then the pH value adding 190kg manganese hydrogen sodium regulating solution is 6.0-7.0, obtain sodium camphorsulfonate feed liquid, setting inlet temperature 130 DEG C, atomization frequency 8000rpm, air outlet temperature is 60 DEG C, the flow velocity of feed control peristaltic pump is 40rpm, with this understanding sodium camphorsulfonate feed liquid is carried out spraying dry, sodium camphorsulfonate product.
Embodiment 2
By 500kg camphorsulfonic acid, 1500kg pure water adds in reactor, 65 DEG C are warming up under stirring, dissolve completely in backward solution and add 15kg gac, leave standstill decolouring 30 ~ 60min, then filtered while hot, filtrate is transferred in the reactor of a cleaning, be heated to 85 DEG C, then the pH value adding 225kg manganese hydrogen sodium regulating solution is 6.0-7.0, obtain sodium camphorsulfonate feed liquid, setting inlet temperature 135 DEG C, atomization frequency 9000rpm, air outlet temperature is 75 DEG C, the flow velocity of feed control peristaltic pump is 45rpm, with this understanding sodium camphorsulfonate feed liquid is carried out spraying dry, sodium camphorsulfonate product.
Embodiment 3
By 500kg camphorsulfonic acid, 1750kg pure water adds in reactor, 70 DEG C are warming up under stirring, dissolve completely in backward solution and add 17.5kg gac, leave standstill decolouring 30 ~ 60min, then filtered while hot, filtrate is transferred in the reactor of a cleaning, be heated to 90 DEG C, then the pH value adding 240kg manganese hydrogen sodium regulating solution is 6.0-7.0, obtain sodium camphorsulfonate feed liquid, setting inlet temperature 140 DEG C, atomization frequency 9500rpm, air outlet temperature is 80 DEG C, the flow velocity of feed control peristaltic pump is 50rpm, with this understanding sodium camphorsulfonate feed liquid is carried out spraying dry, sodium camphorsulfonate product.
Embodiment 4
By 500kg camphorsulfonic acid, 2000kg pure water adds in reactor, 80 DEG C are warming up under stirring, dissolve completely in backward solution and add 20kg gac, leave standstill decolouring 30 ~ 60min, then filtered while hot, filtrate is transferred in the reactor of a cleaning, be heated to 95 DEG C, then the pH value adding 260kg manganese hydrogen sodium regulating solution is 6.0-7.0, obtain sodium camphorsulfonate feed liquid, setting inlet temperature 145 DEG C, atomization frequency 10000rpm, air outlet temperature is 85 DEG C, the flow velocity of feed control peristaltic pump is 55rpm, with this understanding sodium camphorsulfonate feed liquid is carried out spraying dry, sodium camphorsulfonate product.
Claims (5)
1. a production method for dextrocamphoric acid sodium, is characterized in that: it comprises the following steps:
Camphorsulfonic acid is added in purified water, 60 ~ 80 DEG C are warming up under stirring, dissolve completely in backward solution and add gac, leave standstill decolouring 30 ~ 60min, then filtered while hot, filtrate is transferred in the reactor of a cleaning, be heated to 80 ~ 95 DEG C, the pH value then adding manganese hydrogen sodium regulating solution is 6.0-7.0, obtains sodium camphorsulfonate feed liquid, sodium camphorsulfonate feed liquid is carried out spraying dry, sodium camphorsulfonate product.
2. the production method of a kind of dextrocamphoric acid sodium as claimed in claim 1, is characterized in that: described camphorsulfonic acid and the weight ratio of purified water are 1: 0.5-5.
3. the production method of a kind of dextrocamphoric acid sodium as claimed in claim 1, is characterized in that: the consumption of described gac is 2 ~ 5% of camphorsulfonic acid quality.
4. the production method of a kind of dextrocamphoric acid sodium as claimed in claim 1, is characterized in that: described sodium bicarbonate quality is the 0.38-0.55 of camphorsulfonic acid quality.
5. the production method of a kind of dextrocamphoric acid sodium as claimed in claim 1, it is characterized in that: described spray-dired condition is inlet temperature 130-150 DEG C, atomization frequency 8000-10000rpm, air outlet temperature is 60-85 DEG C, and the flow velocity of feed control peristaltic pump is 40-60rpm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410732813.XA CN104402708A (en) | 2014-12-07 | 2014-12-07 | Production method for sodium camphorate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410732813.XA CN104402708A (en) | 2014-12-07 | 2014-12-07 | Production method for sodium camphorate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104402708A true CN104402708A (en) | 2015-03-11 |
Family
ID=52640391
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410732813.XA Pending CN104402708A (en) | 2014-12-07 | 2014-12-07 | Production method for sodium camphorate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104402708A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109912466A (en) * | 2017-12-12 | 2019-06-21 | 武汉武药制药有限公司 | A method of recycling camphorsulfonic acid |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1306530A (en) * | 1998-04-25 | 2001-08-01 | 史密丝克莱恩比彻姆有限公司 | Paroxetine 10-camphorsulfonate for treament of CNS disorders |
-
2014
- 2014-12-07 CN CN201410732813.XA patent/CN104402708A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1306530A (en) * | 1998-04-25 | 2001-08-01 | 史密丝克莱恩比彻姆有限公司 | Paroxetine 10-camphorsulfonate for treament of CNS disorders |
Non-Patent Citations (2)
| Title |
|---|
| 韩丽: "《实用中药制剂新技术》", 30 November 2002 * |
| 韩长日等: "《精细有机化工产品生产技术手册》", 30 June 2010 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109912466A (en) * | 2017-12-12 | 2019-06-21 | 武汉武药制药有限公司 | A method of recycling camphorsulfonic acid |
| CN109912466B (en) * | 2017-12-12 | 2022-01-11 | 武汉武药制药有限公司 | Method for recovering camphorsulfonic acid |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101659635A (en) | Preparation method of methyl p-tolyl sulfone | |
| CN107488130A (en) | A kind of preparation method of lauroyl lysine | |
| CN104130198B (en) | 2-amino-4,6-dimethoxypyridin and preparation method thereof | |
| CN109053535A (en) | A kind of preparation method of n-acetyl-5-methoxytryptamine | |
| CN104402708A (en) | Production method for sodium camphorate | |
| CN102367238A (en) | Method for synthesizing accelerator N,N-dicyclohexyl-2-benzothiazole sulfenamide | |
| CN104496825B (en) | The preparation method of 2-fluorine ethylamine hydrochloride | |
| CN103524450A (en) | Synthetic method for accelerator DZ by using methanol as solvent | |
| CN110526870A (en) | A kind of preparation method of eltrombopag olamine | |
| CN104496833B (en) | A kind of synthesis technique of gabapentin | |
| CN104402881B (en) | A kind of synthetic method of 3-aldehyde radical-6-bromine imidazo [1,2-a] pyridine-8-ethyl formate | |
| CN104447290B (en) | A kind of method preparing 2,4 dichlorophenoxyacetic acid | |
| CN110590564B (en) | Method for synthesizing 2, 4-dichloroaniline by continuous chlorination process | |
| CN104529751B (en) | Preparing method of crystal L-calcium lactate | |
| CN102718681A (en) | Method for purifying yellowed benzophenone hydrazone | |
| CN106967087A (en) | The preparation technology of mezlocillin sodium | |
| CN104513251A (en) | Nalmefene hydrochloride preparation method | |
| CN104447610A (en) | Preparation method for high-purity ethyl 2-(2-aminothiazole-4-yl)-2-(1-tert-butoxycarbonyl-1-methylethoxyimino)acetate | |
| CN106892805B (en) | Synthesis method of 4- (4-hydroxyphenyl) cyclohexanone | |
| CN104557736A (en) | Purification method of sulfadoxine | |
| CN110922345B (en) | Synthesis method of fudosteine | |
| CN105585427A (en) | Method for preparing high-purity ethyl alcohol | |
| CN104529847A (en) | Method for producing methomyl | |
| WO2018094756A1 (en) | Process for producing triethyl citrate | |
| CN103980140A (en) | Abalone shell sourced calcium glutamate and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150311 |