FIELD: chemistry.
SUBSTANCE: invention relates to an improved method of producing 2,7-bis-[2-(diethylamino)ethoxy]-fluorenone-9 dihydrochloride, having immunomodulating properties and a wide range of antiviral action. The method of producing 2,7-bis-[2-(diethylamino)ethoxy]-fluorenone-9 dihydrochloride involves sulphonation of fluorene, oxidative hydroxylation of a disodium salt of 2,7- fluorene disulphonic acid, cyclisation of 4,4'-dihydroxydiphenyl-2-carboxylic acid, alkylation of 2,7-dihydroxyfluorenone with treatment of the obtained alkylated product with concentrated hydrochloric acid. The obtained product undergoes solvent refining through re-extraction of the alkylated product in an aqueous solution treated with hydrochloric acid to obtain a chloride salt of 2,7-bis-[2-(diethylamino)ethoxy]-fluorenone-9, from which nonpolar impurities are washed off using toluene solution and after treatment with alkali, the obtained phases are separated with extraction of 2,7-bis-[2-(diethylamino)ethoxy]-fluorenone-9 into an organic phase. The latter is washed with water in order to remove polar impurities and the product is converted to a chloride salt by treatment with concentrated hydrochloric acid in molar ratio 1:3.5-1:4. Said extraction steps can be carried 1-3 times.
EFFECT: method enables to cut the number of process operations at the purification step, cut solvent consumption and obtain a high-quality product with 99,85-99,90% content of basic substance.
1 tbl, 1 ex
Title | Year | Author | Number |
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2,7-BIS[2-(DIETHYLAMINO)ETHOXY]FLUORENONE DIHYDROCHLORIDE (AMIXIN) PRODUCTION PROCESS | 2006 |
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RU2317974C1 |
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RU2218327C2 |
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METHOD OF PRODUCING DYE ISOSULFAN BLUE (4-{[4-DIETHYLAMINO)PHENYL](2,5-DISULFOPHENYL)METHYLIDENE}-N,N-DIETHYLCYCLOHEXA-2,5-DIENE-1-IMINIUM) | 2023 |
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Authors
Dates
2012-03-10—Published
2010-10-18—Filed