FIELD: chemistry.
SUBSTANCE: invention relates to an improved method of producing 2,7-bis-[2-(di-ethylamino)ethoxy]-fluorenone-9 dihydrochloride, having immunomodulatory properties and a wide range of antiviral action. Method involves sulphonation of fluorene, oxidative hydroxylation of a disodium salt of 2,7-fluorendisulphonic acid, cyclisation of obtained 4,4'-dihydroxydiphenyl-2-carboxylic acid, alkylation of 2,7-dihydroxyfluorenone with hydrochloride with 2-diethylaminoethylchloride to obtain a base which is converted to dihydrochloride. Distinctive feature of the proposed method is that sulphonation of fluorene is carried out with chlorosulphonic acid in molar ratio of fluorene : chlorosulphonic acid of 1:2.2–1:2.3, in temperature range of 0–10 °C with subsequent separation of sodium salt of monosulphofluorene by neutralization of aqueous solution of sulphonation products with sodium hydroxide to pH 8–9 and separation of disodium salt of 2,7-disulfofluorene by evaporation of the obtained filtrate.
EFFECT: method increases output of end product to 36–38 % with respect to initial fluorene and content of basic substance of more than 99 %; wherein amount of by-products is reduced.
1 cl, 2 dwg, 2 ex
Title | Year | Author | Number |
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Authors
Dates
2019-11-25—Published
2019-08-06—Filed