FIELD: chemistry.
SUBSTANCE: improved method of producing 2,7-bis[2-(diethylamino)ethoxy]fluoren-9-one dihydrochloride, known as thylorone or amixine, and used as an immunostimulating and antiviral agent, involves treating 2,7-bis[2-(diethylamino)ethoxy]fluoren-9-one in methylene chloride with hydrogen chloride in gaseous state of in form of hydrochloric acid, preferably in molar ratio 2,7-bis[2-(diethylamino)ethoxy]fluoren-9-one : hydrochloric acid equal to 1:2.05-3.0. A solution of 2,7-bis[2-(diethylamino)ethoxy]fluoren-9-one dihydrochloride in methylene chloride is obtained, which is cooled to temperature not below minus 12°C to obtain a suspension and then filtered and dried. The filtered residue is dried in inert gas or air at temperature from 90 to 110°C or in a vacuum, as a rule. Completion of salt formation is usually controlled from increase in temperature of the reaction mass and its stabilisation to a value between 32 and 34°C, as well as from the pH value, which must not be higher than 4.0. The filtered residue is dried in an inert gas or air, at temperature from 90 to 110°C or in a vacuum, as a rule.
EFFECT: simplification of the process due to exclusion of inflammable solvents and obtaining a product of high quality with high output.
6 cl, 1 dwg, 3 ex
Title | Year | Author | Number |
---|---|---|---|
CRYSTALLINE FORM IV OF TILORONE DIHYDROCHLORIDE, AND INDUSTRIAL METHOD FOR ITS PRODUCTION (VERSIONS) | 2012 |
|
RU2509074C2 |
2,7-BIS[2-(DIETHYLAMINO)ETHOXY]FLUORENONE DIHYDROCHLORIDE (AMIXIN) PRODUCTION PROCESS | 2006 |
|
RU2317974C1 |
METHOD FOR PREPARING 2,7-BIS-[2-(DIETHYLAMINO)- ETHOXY]FLUORENONE-9 DIHYDROCHLORIDE AS ANTIVIRAL AND IMMUNOMODULATION PREPARATION "AMIXINUM" | 1999 |
|
RU2218327C2 |
METHOD OF PRODUCING 2,7-BIS[2-(DIETHYAMINO)ETHOXY]-FLUORENONE-9 DIHYDROCHLORIDE | 2010 |
|
RU2444512C1 |
METHOD OF PRODUCING 2,7-BIS-[2-(DIETHYLAMINO)ETHOXY]-FLUORENONE-9 DIHYDROCHLORIDE | 2019 |
|
RU2707176C1 |
METHOD FOR PRODUCTION OF 2,7-BIS[2-(DIETHYLAMINO0ETHOXY]FLUORENONE DIHYDROCHLORIDE | 1994 |
|
RU2076097C1 |
CRYSTALLINE FORM II OF TILORONE AND METHOD OF OBTAINING THEREOF (VERSIONS) | 2011 |
|
RU2521595C2 |
DRUG PREPARATION TILORONE IN SUPPOSITORIES | 2008 |
|
RU2411032C2 |
PERORAL MEDICINE TILORONE | 2007 |
|
RU2336073C1 |
METHOD FOR PREPARING ANTIVIRAL PREPARATION AMIXINUM (TILORONE DIHYDROCHLORIDE) (VARIANTS) | 2000 |
|
RU2216344C2 |
Authors
Dates
2009-12-10—Published
2008-05-23—Filed