CS215374B1 - Process for the production of pei-acetylsalicylotrialuininium dioxide - Google Patents
Process for the production of pei-acetylsalicylotrialuininium dioxide Download PDFInfo
- Publication number
- CS215374B1 CS215374B1 CS539880A CS539880A CS215374B1 CS 215374 B1 CS215374 B1 CS 215374B1 CS 539880 A CS539880 A CS 539880A CS 539880 A CS539880 A CS 539880A CS 215374 B1 CS215374 B1 CS 215374B1
- Authority
- CS
- Czechoslovakia
- Prior art keywords
- aluminum
- dioxide
- product
- propanoate
- added
- Prior art date
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
Vynález sa týká spósobu výroby pentaacetylsalicylotrialuminiumdioxidu (Aloxiprínu), ktorý jfe surovinou pre farmaceutické výrobky. Vynález rieši přípravu uvedenej substancie v kvalitě, výhovujúcej požiadavkám liekopisu. Podstata spočívá v tom, že sa před izoláciou produktu analyticky stanoví v ňom množstvo zhydrolyzovanej kyseliny acetylosalicylovej a přidá sa na každé 0,1 % stánovenej kyseliny salicylovej 100 g 2-propanolátu hlinitého.The invention relates to a method for producing pentaacetylsalicylotrialuminiumdioxide (Aloxiprin), which is a raw material for pharmaceutical products. The invention provides for the preparation of the said substance in a quality that meets the requirements of the pharmacopoeia. The essence lies in the fact that before isolating the product, the amount of hydrolyzed acetylsalicylic acid is analytically determined in it and 100 g of aluminum 2-propanolate is added for every 0.1% of the stannous salicylic acid.
Description
Vynález sa týká sposobu výroby farmaceutickej substancie pentaacetylsalicylotrialummiumdioxidu (Aloxiprínu) liekopisnej kvality.The present invention relates to a process for the manufacture of a pharmaceutical substance of pentaacetylsalicylotrialummium oxide (Aloxiprine) of pharmaceutical quality.
Pentaacetylsalicylotrialuminiumdioxid sa připravuje reakciou kyseliny acetylosalicylovej s 2-propanolátom hlinitým za přítomnosti rozpúšťadiel (2-propanol, aceton) a za pridania vody.podra schématu:Pentaacetylsalicylotrialuminium dioxide is prepared by reacting acetylsalicylic acid with aluminum 2-propanoate in the presence of solvents (2-propanol, acetone) and adding water.
ococh3 ococh 3
A/A /
3[(CH3)2CH—O]3A1 + 5 || +3 [(CH 3 ) 2 CH-O] 3 A1 + 5 || +
+ 9(CH3)2CH—OH.+ 9 (CH 3 ) 2 CH-OH.
Po skončení reakcie sa vzniklá substancia odsaje, premyje a vysuší. V priebehu reakcie a pri dalšom spracovaní vzniká následkom hydrolýzy kyseliny acetylosalicylovej kyselina salicylová, ktorá je v konečnom produkte nežiadúca.After completion of the reaction, the resulting substance is filtered off with suction, washed and dried. During the reaction and further processing, the hydrolysis of acetylsalicylic acid produces salicylic acid, which is undesirable in the final product.
Autoři vynálezu zistili, že pri príprave tejto soli je dóležitým faktorom, ktorý ovplyvňuje kvalitu vyrobenej substancie, množstvo pridávanej reakčnej vody. Ide o malé množstvo vody, z ktorej převážná část je priamo přítomná v použitých rozpúšťadlách. Přesné stanovenie tejto vody je pri súčasnom stave analytických metod obtiažne (najma v acetone). Přitom už malý nadbytok vody spósobuje hydrolýzu kyseliny acetylosalicylovej a přítomnost kyseliny salicylovej v konečnom produkte. Nedostatok vody sposobuje, že časť kyseliny acetylosalicylovej nezreaguje s 2-propanolátom hlinitým, čo tiež sposobuje zníženie kvality produktu. Nadbytok 2-propanolátu hlinitého spósobi, že v konečnom produkte sú látky, nerozpustné v dimetylformamide a produkt nevyhovuje požiadavkám liekopisu.The inventors have found that the amount of reaction water added is an important factor affecting the quality of the substance produced in the preparation of this salt. This is a small amount of water, most of which is directly present in the solvents used. Accurate determination of this water is difficult in the current state of analytical methods (especially in acetone). Even a small excess of water causes the hydrolysis of acetylsalicylic acid and the presence of salicylic acid in the final product. The lack of water causes part of the acetylsalicylic acid not to react with aluminum 2-propanoate, which also causes a decrease in product quality. Excess aluminum 2-propanoate causes the final product to be insoluble in dimethylformamide and the product does not meet the requirements of the pharmacopoeia.
Tento nedostatok odstraňuje vynález, podťa ktorého sa v pripravenom Aloxipríne před jeho izoláciou analyticky stanoví množstvo zhydrolyzovanej kyseliny acetylosalicylovej a přidá sa na každé stanovené 0,1 % (hmot. množstvo) zhydrolyzovanej kyseliny acetylosalicylovej 100 g 2-propanolátu hlinitého, čím sa dosiahne, že výsledný produkt je vyhovujúcej kvality.This drawback removes the invention according to which the amount of hydrolysed acetylsalicylic acid is analytically determined in the prepared Aloxiprine prior to its isolation and 100 g of aluminum 2-propanolate is added to each determined 0.1% (w / w) of the hydrolysed acetylsalicylic acid, thereby ensuring that the resulting product is of satisfactory quality.
Ďalej uvedený příklad ilustruje spósob přípravy podlá vynálezu:The following example illustrates the preparation method of the invention:
Do smaltovaného kotlá sa našaržuje 140 1 2-propanolu a 70 1 acetonu. Vyhřeje sa na 50 °C, přidá sa 102,9 kg kyseliny acetylosalicylovej. Potom sa přidá vypočítané množstvo vody. Z odmerky sa připustí 70 kg 2-propanolátu hlinitého, pričom vypadává pentaacetylsalicylotrialuminiumdioxid. Nakoniec sa přidá k reakčnej zmesi 70 1 2-propanolu, vymieša sa 1/2 hodiny, odoberie sa cca 20 g vzorky, ktorá sa odsaje, premyje 2-propanolom a vysuší. Vo vzorke sa stanoví obsah volnej kyseliny salicylovej. Podía zisteného množstva sa přidá na každé 0,1% volnej kyseliny salicylovej 100 g 2-propanolátu hlinitého, vymieša sa pri 50°C 1/2 hodiny, izoluje sa, premyje a suší. Získá sa produkt, vyhovujúei požiadavkám liekopisu.140 l of 2-propanol and 70 l of acetone are charged into an enamelled boiler. Heat to 50 ° C, add 102.9 kg acetylsalicylic acid. The calculated amount of water is then added. 70 kg of aluminum 2-propanoate are allowed to form pentaacetylsalicylotrialuminium dioxide. Finally, 70 l of 2-propanol are added to the reaction mixture, mixed for 1/2 hour, about 20 g of sample are taken, which is suctioned off, washed with 2-propanol and dried. The free salicylic acid content is determined in the sample. According to the amount determined, 100 g of aluminum 2-propanoate are added to each 0.1% of free salicylic acid, mixed at 50 ° C for 1/2 hour, isolated, washed and dried. A product is obtained which meets the requirements of the pharmacopoeia.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS539880A CS215374B1 (en) | 1980-08-05 | 1980-08-05 | Process for the production of pei-acetylsalicylotrialuininium dioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS539880A CS215374B1 (en) | 1980-08-05 | 1980-08-05 | Process for the production of pei-acetylsalicylotrialuininium dioxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CS215374B1 true CS215374B1 (en) | 1982-08-27 |
Family
ID=5398811
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS539880A CS215374B1 (en) | 1980-08-05 | 1980-08-05 | Process for the production of pei-acetylsalicylotrialuininium dioxide |
Country Status (1)
| Country | Link |
|---|---|
| CS (1) | CS215374B1 (en) |
-
1980
- 1980-08-05 CS CS539880A patent/CS215374B1/en unknown
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| SU731879A3 (en) | Method of synthetic tobacco production | |
| CH614950A5 (en) | Process for the preparation of 5-methylisoflavones | |
| CS215374B1 (en) | Process for the production of pei-acetylsalicylotrialuininium dioxide | |
| SU555857A3 (en) | Method for preparing 3-oxo17-n-amyloxyestra-4,9,11-triene | |
| SU865787A1 (en) | Method of producing yttrium orthophosphate dihydrate | |
| EP0341478A3 (en) | Method for the preparation of 2,3-dichloro-5-acetyl pyridine | |
| SU670571A1 (en) | Method of producing 3-methyl-1-phenyl-4-hydrozone of pyrazol-4,5-dione | |
| RU2033402C1 (en) | Method of preparing of phosphate binder | |
| FR2297832A1 (en) | PROCESS FOR PREPARING ESTERS FROM FORMIC ACID | |
| JPS5851000B2 (en) | Production method of sulfolitocholylglycyltyramine | |
| SU442185A1 (en) | Method for Producing Modified Starch | |
| DE1915827C3 (en) | Process for the production of acidic ion exchangers based on agarose | |
| DE525403C (en) | Process for the preparation of water-soluble condensation products of aminoarylarsine oxides | |
| DE958924C (en) | Process for the preparation of mercury-containing dioxypropane compounds | |
| SU979326A1 (en) | Process for producing calcium salts of higher carboxylic acids | |
| DE116645C (en) | ||
| SU423181A1 (en) | METHOD OF OBTAINING CHARGE FOR FERRITES | |
| SU1038337A1 (en) | Process for preparing diethyl ether of itaconic acid | |
| SU1477729A1 (en) | Method of producing 4-hydroxy-8-carboxyquinolone-2 | |
| SU777032A1 (en) | Method of preparing 2,6-dimethyl-4-arylvinylpyrylyl salts | |
| US4078140A (en) | 2,3-Di-(2,3-diiodopropoxy)-propyl cellulose and method of producing the same | |
| SU451689A1 (en) | The method of obtaining nitromezitilen | |
| SU133882A1 (en) | Method for preparing naphthylene-1,5-bis-dialkyl esters of amidophosphono-formic acid | |
| SU721101A1 (en) | Gyndarine producing method | |
| SU730449A1 (en) | Paste for eliminating casting-core flaws |