2,7-bis[2-(diethylamino)ethoxy]fluorenone dihydrochloride (amixin) production process

FIELD: industrial organic synthesis.

SUBSTANCE: invention provides improved 2,7-bis[2-(diethylamino)ethoxy]fluorenone dihydrochloride production process comprising stages of sulfurization of fluorenone followed by neutralization of obtained reaction mass, isolation of purified fluorenone-2,7-disulfonic acid disodium salt, "alkaline melting" of this salt in presence of sodium nitrate to form 4.4'-dihydroxydiphenyldicarboxylic acid, cyclization to form 2,7-dihydroxyfluorene and alkylation thereof. More specifically, 2,7-dihydroxyfluorene obtained in cyclization stage is converted into alkali metal salt and toluene solution of 2-diethylaminoethyl chloride is added to preheated aqueous solution of the above salt at molar ratio 1:(3-5), preferably 1:4, to form 2,7-bis[2-(diethylamino)ethoxy]fluorenone, which is then treated with concentrated aqueous hydrochloric acid at molar ratio 1:(3.5-4), preferably 1:3.5.

EFFECT: increased yield and improved quality of product, and simplified process.

3 cl, 3 dwg, 4 ex

 

The invention relates to the field of organic chemistry, and in particular to an improved process for the preparation of the dihydrochloride of 2,7-bis[2-(diethylamino)ethoxy]fluorenone(Amiksin) of the formula I:

which is now widely used in medical practice as an antiviral and immunostimulating substance /Biol. Unteract. 1987, v.62, No.1, p.25-42, RF patent 2122425, 27.11.1998, patent RF, 20.11.1999/.

There are a number of ways to obtain 2,7-bis[2-(diethylamino)ethoxy]fluorenone dihydrochloride (I)on the basis of fluorene (II).

One of them /M.Burke Sister, Medeleine M.Joulie "New synthetic pathways to tilorone hydrochloride", Synthetic Com. 1976, 6(5), p.371-376/ is that fluoren in turn derived fluorenone by acetylation acetyl chloride in the presence of aluminum chloride by the reaction of the Friedel-with the formation of 2,7-diacetylene (III), the resulting diacetate oxidized by the Bayer-Wiliger adharmasya acid in a suitable organic solvent with the formation of 2,7-diacetoxy fluorene (IV), which in turn are oxidized by sodium bichromate in acetic acid with the formation of 2,7-diacetoxy of fluorenone (V). The resulting compound (V) alkylate the hydrochloride of 2-diethylaminoethylamine in a mixture of toluene-aqueous solution of potassium hydroxide in the presence of benzyltriethylammonium bromide as catalyst, meifa the aqueous migration the organic layer was separated, washed with water and saturated sodium chloride solution, dried with anhydrous magnesium sulfate, filter drier, evaporated the solution to dryness, the residue dissolved in methanol and treated with dry hydrogen chloride in diethyl ether. After recrystallization from methanol-isopropanol get the target product 2,7-bis[2-(diethylamino) ethoxy]fluorenone the dihydrochloride (I) 50% of the output stage alkylation and with a total output of 10%, see diagram:

Another way to obtain 2,7-bis[2-(diethylamino)ethoxy]fluorenone dihydrochloride (I) /Patent RF 2076097, 27.03.1997/ is that obtained from fluorene (II) fluorene (VI) is dissolved in glacial acetic acid and treated by heating with iodine in the presence of a mixture of sulfuric and nitric acids obtained 2,7-diiodofluorescein (VII) is treated with 2-diethylamino-ethylate and potassium in the presence of 18-crown-6 in a medium dry dimethylformamide or dioxane. The allocation of 2,7-bis[2-(diethylamino)ethoxy]fluorenone lead by diluting the reaction mixture with water, separating by filtration the precipitate-base, wash it with water, suspendirovanie in the water by sedimentation of concentrated hydrochloric acid, drying the target product - 2,7-bis[2-(diethylamino)ethoxy]fluorenone dihydrochloride (I) with 72% yield under alkylation and 24% of total output, see diagram:

According to another method /JP 9031036, 04.02.1997/ obtained by the oxidation of fluorene the bichromate in acetic acid fluorenone (VI) nitrous by a mixture of nitric and sulfuric acids with the formation of 2,7-dinitrofluorene (VIII), which restores tin chloride or hydrogen in the presence of Lindlar catalyst (10% palladium), poisoned 5% of lead at a pressure of 40-60 kg/cm2obtained a suspension of 2,7-diaminofluorene (IX) 50% terraforming acid diasterous the sodium nitrite, filtered explosive salt, page (X), which in turn is metered in boiling 50% sulfuric acid with the formation of 2,7-doxifluridine (XI). The compound (XI) alkylate the hydrochloride of 2-diethylaminoethylamine in a mixture teleology solution of potassium hydroxide, separating the organic layer containing 2,7-bis[2-(diethylamino)ethoxy]fluorene, washed with water and saturated sodium chloride solution, dried with anhydrous magnesium sulfate, filter drier, evaporated the solution to dryness, the residue is dissolved in isopropanol, treated with a solution of hydrogen chloride in ethanol and receive 2,7-bis[2-(diethylamino)ethoxy]fluorenone the dihydrochloride (I) 50% output (at the stage of alkylation) and the total output is 11%, see diagram:

All of the above ways to get on the hydrochloride 2,7-bis [2-(diethylamino)ethoxy]fluorenone (I) are characterized by low total output, insufficient quality of the target product (TPL 235-236°C)significant consumption of solvents, the use of hard, expensive and toxic reagents. All this makes these methods multihelical and not suitable for use in industrial production.

More sophisticated in design and allows to obtain the target product dihydrochloride 2,7-bis[2-(diethylamino)ethoxy]fluorenone (I) in good yield is a method of obtaining dihydrochloride 2,7-bis/2-(diethylamino)ethoxy/fluorenone /Owijarki, Aigrain, Logicview and other DAN USSR, ser. Geology, Chemistry, Biology, science, 1976, No. 7, str-611/, which is the sulfonation of fluorene low-interest-oleum, the allocation of disodium salt 2,7-disulfonate fluorene(UE) fractional crystallization of the mixture of water, alkali melting of this salt in terms of heating it at 270-275°With 5 moles of caustic soda in the presence of sodium nitrate for 8 hours. The resulting reaction after blanking and acidification of alkaline water 50%sulfuric acid, 4,4'-dihydroxy-2-biphenylcarbonic acid (IX) is subjected to reaction cyclodehydration when vzimodejstviyu with zinc chloride at 200-210°C, resulting in the formation of 2, 7-dihydroxyflavone (VI), which is subjected to alkylation in the interaction with 2.5 moles hydrochloride 2-diet is aminoacylated in two-phase environment, toluene-water, in the presence of sodium hydroxide and catalytic amounts of trimethylphenylammonium bromide boiling within 24 hours. Then separate the organic layer evaporated it to dryness, dissolve the residue in methanol and the resulting solution was treated with saturated hydrogen chloride in sulphuric ether and precipitated residue is recrystallized from a mixture of ethanol: isopropanol 1:3 receive with the release of 50% of the dihydrochloride of 2,7-bis-/2-(diethylamino)ethoxy/fluorenone-9 ("Amiksin", I). The total yield of the target product is 28.8%, TPL 235-235°C. the Disadvantages of this method are: the duration of the synthesis, a huge number trudnoozhidaemyh acidic waste, low quality target product.

Closest to the proposed method is described in the patent of the Russian Federation 2218327, 10.12.2003, consisting in the sulfonation of fluorene sulfuric acid density of 1.83-1.84 g/cm3at a temperature of 160-165°C for 20 minutes, diluted with water and neutralizing with caustic soda to a pH of 4-4 .5 mixture of sulphonic acids, the allocation of purified disodium salt 2,7-disulfonate fluorene (VII) by recrystallization of this mixture from the water, after which the latter is subjected to the reaction of alkaline melting by heating for 2.5-3 hours at 220-230°with sodium hydroxide in the presence of catalytic amounts of ammonia water and a mixture of nitric acid and sodium nitrite potassium in atih in a weight ratio to each other 5:1. Formed after quenching alkaline water and acidification of 50%sulfuric acid, 4,4'-dihydroxy-2-biphenylcarbonic acid (IX, yield 88%) when heated at a temperature of 200-205°C for 30 minutes, turn the 2.7-dihydroxyflavone (VI, yield 90%). Then, the obtained fluorine (VI) is subjected to alkylation reaction by interaction with 2.5 to 3 moles of the hydrochloride of 2-diethylaminoethylamine boiling for 20 hours in toluene with 40%sodium hydroxide solution. Formed the basis of the "Amiksin" - 2,7-bis-/2-(diethylamino)ethoxy/fluorene-9 (I) is dissolved in acetone and converted into "Amiksin" - dihydrochloride 2,7-bis-/2-(diethylamino)ethoxy/fluorene-9 (I) by adding 35%hydrochloric acid in acetone solution of the base of "Amiksin". Total yield "Amiksin" - 32-34%, considering the original fluoren (II), at alkylation - 57%, TPL 233-235°C. However, this method of obtaining the dihydrochloride 2,7-bis-/2-(diethylamino)ethoxy/fluorenone-9 has several disadvantages.

First of all, it requires strict compliance with the conditions of the process. Changing conditions in one direction or another can lead to reduced yield of the target product, reducing its quality. For example, the use of sulfuric acid density below to 1.83 g/cm3leads to lower output of the disodium salt 2,7-disulfonate fluorene (VII), and the increase in density used is islote above 1.84 g/cm 3without increasing the yield of the target product, results in excessive sulfureuse agent and increase the acidic effluent reduction temperature the reaction of alkaline melting point below 210°leads to reduction of the yield of reaction product and a significant amount of time conducting the synthesis, increasing the reaction temperature alkaline melting above 230-280°does not contribute to increase the yield of the final product, and increases the power consumption by carrying out the reaction and, thereby, increases the cost of the target product. The process of alkylation of 2.7-dihydroxyflavone includes a distillation of the toluene solution almost to dryness, requires a significant consumption of volatile solvents of hexane and acetone. In addition, it is complicated by the occurrence of adverse reactions of 2-diethylaminoethylamine in basic environments, which reduces the quality of the target product.

Thus, none of the known methods can not obtain the dihydrochloride 2,7 - bis-/2-(diethylamino)ethoxy/Floreana-9 required quality for more technological scheme of reducing the amount of organic solvents, reducing the possibility of occurrence of adverse reactions.

The task of the invention is to develop a new and improved method of obtaining dihydrochloride 2,7 - bis-/2-(diethylamino)ethoxy/Floreana-9, allowing Powys the th its output, to improve the quality of the target product, to simplify the process of its synthesis and eliminate the use of expensive reagents.

The problem is solved by the proposed method of obtaining dihydrochloride 2,7-bis/2-(diethylamino)ethoxy/fluorenone-9(1), which includes stages of sulfonation of fluorene with subsequent neutralization of the reaction mass and the allocation of purified disodium salt 2,7-disulfonate fluorene, "alkaline melting" of this salt in the presence of nitric acid with the formation of sodium 4,4' dioxideemissions acid, cyclization and alkylation 2,7-doxifluridine, namely that obtained by the cyclization stage 2,7-dioxypurine transformed into a salt of an alkali metal and a preheated aqueous solution of this salt add toluene solution 2-diethylaminoethylamine at a molar ratio of 1:3-1:5, preferably 1:4, obtained 2,7-bis/2-(diethylamino)ethoxy fluorine treated with concentrated hydrochloric acid in a molar ratio of 1:3.5 to 1:4, preferably of 1:3.5.

The proposed method allows to obtain the target product with TPL 237-238°With a total yield of about 50-55%, the output stage alkylation - 95%.

Comparison of the proposed method to obtain dihydrochloride 2,7-bis[2-(diethylamino)ethoxy]fluorenone (I), with analogues showed that it is not known technical is some solution of the problem, which would place the proposed combination of signs, which would give the specified result.

Change order dosage does not achieve the target, on the contrary, the output dihydrochloride 2,7-bis[2-(diethylamino)ethoxy]fluorenone (I) is even decreasing. Also does not increase the output of the dosage of the hydrochloride of 2-diethylaminoethylamine. Such an unexpected result, as it turned out, is associated with the occurrence of adverse reactions of 2-diethylaminoethylamine in basic environments. Dosage toluene solution of 2-diethylaminoethylamine allows you to comprehensively carry out the alkylation reaction, to greatly reduce the amount of impurities to move product dosage to a toluene solution of 2,7-bis[2-(diethylamino)ethoxy]fluorenone of concentrated hydrochloric acid. Base - 2,7-bis[2-(diethylamino)ethoxy]fluorene dissolved in stoichiometric quantity of concentrated hydrochloric acid and does not precipitate during the long term ageing at low temperature and the introduction of the seed. The dihydrochloride of 2,7-bis[2-(diethylamino)ethoxy]fluorenone (I) is emitted during the evaporation of the water-toluene mixture, during which separates the water in the form of an azeotropic mixture and crystallization of the desired product. Using such method of selection for methods with lower output prevadid education oily, rather than crystalline product, highly contaminated with impurities, including unreacted 2,7-doxifluridine (according to TLC, HPLC).

Only offer a set of distinctive from the nearest technical solutions features allows you not only to increase the output stage alkylation and quality of the target product, but, in General, significantly improve the manufacturability of the process of obtaining dihydrochloride 2,7-bis[2-(diethylamino)ethoxy]fluorenone, and it gives the basis to consider the proposed method as inventive.

Information confirming the possibility of implementing the method shown in the following examples. Subjected to alkylation 2,7-dioxypurine get from fluorene under the conditions described in the patent of the Russian Federation 2218327.

Example 1

To a degassed solution of 34 g of potassium hydroxide (or 24 g of sodium hydroxide in 200 ml of water under a stream of nitrogen sprinkled of 63.6 g of 2,7-doxifluridine (0.3 mol), maintained under stirring for 15 minutes and get water solution to 86.4 g of Pikalevo salt 2,7-doxifluridine (with 76.8 g of disodium salt 2,7-doxifluridine). To the resulting solution was heated to 82-85°C for 15 h, dispense the solution 163,8 g (1.2 mol) of 2-diethylaminoethylamine in 900 ml of toluene. After dosing the reaction mass incubated for another 5 hours, the Reaction mixture was separated, toluol the initial solution washed with water (100 ml) and treated with 93 g of 35% hydrochloric acid. The mixture is evaporated before the termination of allocation of water (in the form of an azeotropic mixture of toluene-water), cooled to room temperature and filtered receive 137,8 g (95% of theory) of the dihydrochloride of 2,7-bis[2-(diethylamino) ethoxy]fluorenone. TPL=237-238°C.

Found25H36Cl2O3: With=62,15%, N=7,50%, N=Of 5.82%, Cl=14,5%.

Calculated: C=62,11%, N=7,51%, N=5,79%, Cl=14,67%.

NMR spectrum1N (D2): 1,00 ppm (N, t, CH3), of 2.56 ppm (8H, HF, CH2), 2,61, and 4,32 ppm (8H, two m, CH2), 6,00 ppm (2H, USS, ArH-1), to 7.15 ppm (2H, USD, ArH-3), 7,00 ppm (2H, USD, ArH-4).

NMR spectrum13With (D2O): 7,3 ppm (CH3), to 49.3 ppm (CH2), and 57.6 ppm (CH2), 71,7 ppm (CH2), 106,9 ppm (CH, Ar-1), 157,4 ppm (S, Ar-2), 117,7 ppm (CH, Ar-3), 120,9 ppm (CH, Ar-4), 191,0 ppm (C=O), 142,4 ppm (S, Ar-10), 134,6 ppm (S, Ar-11).

Examples 2-4

Changing the molar ratio of the salt of 2,7-doxifluridine: diethylaminoethylamine indicates adequacy ratio of 1:4, the reduction does not lead to the achievement of output, the increase does not lead to the improvement of the technical result:

204,8
ExampleNumber of diethylaminoethylamine, gThe molar ratioOutput %
2of 112.81:373
3br143.31:3,584
41:596

Examples 5-7

The influence on the yield of the dihydrochloride of 2,7-bis[2-(diethylamino)ethoxy]fluorenone amount of hydrochloric acid is reflected in the examples:

ExampleQuantity of hydrochloric acid, gThe molar ratioOutput %
5621:272
6108,51:3,596
71241:496

Technological design of the proposed method is much simpler than the nearest equivalent. The allocation now does not include the Stripping of toluene to dryness, does not require the use of hexane and dissolution of the residue in acetone before treatment with concentrated hydrochloric acid. By reducing the total amount of organic solvents increased process safety. Toluene can be used in the process again. Without additional purification send it to the stage of preparation of toluene solution of 2-diethylaminoethylamine. This allows not only to increase the efficiency of the method, but also significantly reduce the amount of organic solvents.

The implementation of this method allows to obtain 2,7-bis[2-(diethylamino)ethoxy]fluorescence is Ortona the dihydrochloride (I) without the use of toxic and expensive reagents while increasing output and technological process, the use of standard equipment and available reagents, therefore, the proposed solution meets the criterion of industrial applicability.

1. The method of obtaining dihydrochloride 2,7-bis[2-(diethylamino)ethoxy]fluorenone-9, which includes stages of sulfonation of fluorine, followed by neutralization of the resulting reaction mass, the allocation of purified disodium salt 2,7-disulfonate fluorene, "alkaline melting" of this salt in the presence of nitric acid with the formation of sodium 4,4'-dioxideemissions acid, cyclization and alkylation 2,7-doxifluridine, characterized in that obtained in the cyclization stage 2,7-dioxypurine transformed into a salt of an alkali metal and a preheated aqueous solution of this salt add toluene solution of 2-diethylaminoethylamine at a molar ratio of 1:3-1:5, and the resulting 2,7-bis[2-(diethylamino)ethoxy]fluorene treated with concentrated hydrochloric acid at a molar ratio of 1:3.5 to 1:4.

2. The method according to claim 1, wherein the pre-heated solution of alkali metal salt of 2,7-doxifluridine add toluene solution of 2-diethylaminoethylamine at a molar ratio of 1:4.

3. The method according to claim 1, wherein the 2,7-bis[2-(diethylamino)ethoxy]fluorene treated with concentrated hydrochloric acid at a mole is th ratio of 1:3.5.



 

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6 cl, 1 dwg, 3 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing and aminophenol compound of formula (1) , where each of R1 and R2, which can be identical or different, are a hydrogen atom, C1-C6 alkyl group, which can be substituted with phenyl, or phenyl; R1 and R2 together with the neighbouring nitrogen atom can form a 5- or 6-member heterocyclic group, selected from piperidinyl and piperazinyl; the heterocyclic group can be substituted with one substitute selected from hydroxyl group, C1-C6 alkyl group and phenoxy group, which can have a C1-C6 alkoxy group, substituted with 1-3 halogen atoms. The method involves reacting a cyclohexanedione compound of formula (2) with a amine compound of formula (3) , where R1 and R2 assume values given above, in neutral or basic conditions.

EFFECT: wider range of use of the compound.

8 cl, 4 dwg, 13 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method for synthesis of 4-(dimethylamino)-1-alkyl-1-methyl-2-alkyn-1-ols of general formula (1): where R=C2H5, C4H9, C6H13, which are substances with physiological activity, particularly cholinolytic properties. The method involves reacting 3-alkyl-3-methyl-1-alkyn-3-ols with N,N,N1,N1-tetramethylmethanediamine in the presence of a copper monochloride catalyst in molar ratio 3-alkyl-3-methyl-1-alkyn-3-ol: N,N,N1,N1-tetramethylmethanediamine: CuCl=10:(10-12):(0.4-0.6) in an argon atmosphere at temperature 50-90C and atmospheric pressure, predominantly at 80C, for 3-5 hours. Output of 4-(dimethylamino)-1-alkyl-1-methyl-2-alkyn-1-ols (1) is 84-96%.

EFFECT: method increases output of products.

1 cl, 3 dwg, 1 tbl, 12 ex

FIELD: chemistry.

SUBSTANCE: invention relates to an improved method of producing 2-[(dimethylamino)methyl]phenol used in the food industry and medicine, as well as lubrication and engine oil additives, corrosion inhibitors for different types of steel, stabilisers of motor car and rocket fuel, monomers, plastic and different types of rubbers. The method involves reacting phenol with N,N,N,N-tetramethylmethylenediamine. The reaction is carried out in the presence of a copper (I) chloride catalyst in molar ratio phenol: N,N,N,N-tetramethylmethylenediamine: CuCl=10:(10-11):(0.2-0.4) at atmospheric pressure, mainly at temperature of 50C for 3.5-4.5 hours.

EFFECT: increased selectivity of the process and output of the desired product, reduced reaction temperature.

1 cl, 2 dwg, 1 tbl, 1 ex

FIELD: medicine, pharmaceutics.

SUBSTANCE: in the given invention, there is offered a method for preparing a compound of formula , where Y is specified of CH3, CH2OH, CH2CH2OH, CH2Br and Br; involving the stages: (1) reaction of the compound of formula where OX represents hydroxy or O-M+ where M+ represents cation chosen of Li+, Na+ and K+ and Y is such as specified above; with trans-cynnamaldehyde , with a secondary amine compound added; then (2) acid treatment of a product from the previous stage to prepare a compound of formula (I). The aforesaid method can be used for preparing tolterodine and fezoterodine which are effective in treating the hyperactive urinary bladder. There are also declared compounds of formulae V, VI and VII.

EFFECT: development of the effective method for preparing the compound.

25 cl, 19 ex

FIELD: industrial organic synthesis.

SUBSTANCE: invention provides improved 2,7-bis[2-(diethylamino)ethoxy]fluorenone dihydrochloride production process comprising stages of sulfurization of fluorenone followed by neutralization of obtained reaction mass, isolation of purified fluorenone-2,7-disulfonic acid disodium salt, "alkaline melting" of this salt in presence of sodium nitrate to form 4.4'-dihydroxydiphenyldicarboxylic acid, cyclization to form 2,7-dihydroxyfluorene and alkylation thereof. More specifically, 2,7-dihydroxyfluorene obtained in cyclization stage is converted into alkali metal salt and toluene solution of 2-diethylaminoethyl chloride is added to preheated aqueous solution of the above salt at molar ratio 1:(3-5), preferably 1:4, to form 2,7-bis[2-(diethylamino)ethoxy]fluorenone, which is then treated with concentrated aqueous hydrochloric acid at molar ratio 1:(3.5-4), preferably 1:3.5.

EFFECT: increased yield and improved quality of product, and simplified process.

3 cl, 3 dwg, 4 ex

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 12C to obtain a suspension and then filtered and dried. The filtered residue is dried in inert gas or air at temperature from 90 to 110C 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 34C, 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 110C 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

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

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