Method of preparing three-component complexes of o-cresoxyacetic and p-chloro-o-cresoxyacetic acid with triethanolamine and biogeneous metals

FIELD: chemistry.

SUBSTANCE: method involves reacting triethanol ammonium salts of o-cresoxyacetic and p-chloro-o-cresoxyacetic acid with the corresponding metal salt in alcohol or aqueous medium preferably at room temperature for 1-48 hours. The three-component complexes are extracted through solvent distillation with subsequent washing of the formed powder with ether and drying in a vacuum. The said complexes can be used as a base for making medicinal drugs.

EFFECT: design of a method of preparing complexes of o-cresoxy- and p-chloro-o-cresoxyacetic acid, triethanolamine and metals having formula n[R(o-CH3)-C6H3-OCH2COO-•N+H(CH2CH2OH)3]•MXm, where R = H, p-Cl; M = Mg, Ca, Mn, Co, Ni, Cu, Zn, Rh, Ag; X = CI, NO3, CH3COO; n = 1, 2; m = 1-3.

2 cl, 11 ex

 

The invention relates to new biologically active compounds from the class of derivatives aryloxyacetic acids and the way they are received and can be used in medicine and biology as the basis for making medicines. Tris(2-hydroxyethyl)ammonium salt of cresoxy- (COOK) and p-chloro-o-resocialising acids (HCUK) General formula:

o-CH3RC6H3OCH2COO-·N+H(CH2CH2OH)3,

where R=H (medicine "traceson"), R=p-Cl (chlorocresols"), have adaptogenic, hemo - and immunomodulatory properties, have antioxidant, membranostabiliziruyuschee and antitumor activity, protect the body in cardiogenic shock, toxic stress, alcohol poisoning, heavy metals, effect of irradiation [1-5].

Biogenic metals play an important role in the vital processes of living organisms: part of enzymes, vitamins, provide the body's need for essential trace elements, are part of the drug [6].

Known [7, 8] bicomponent complexes of salts of these metals with one or two molecules of triethanolamine (tea), which are formed by the coordination of the oxygen atoms of hydroxyl groups and nitrogen atoms with metal type [N(CH2CH2OH)3]n·MX where M=Li, Na, Ba, Cd, Pb, Fe, Ni, etc. X=Cl, ClO4, Br, NO3CH3Soo. n=1, 2. m=2, 3.

Ternary complexes of cresoxy - and p-chloro-o-resocialising acids, tea and metals is not known.

The aim of the present invention is to provide a previously unknown ternary complex compounds on the basis of "trekrezan" and "chlormezanone" and the above-mentioned metals.

The invention consists in developing methods for obtaining a previously unknown type three-component complex compounds consisting of o-cresoxy - and p-chloro-o-resocialising acid, triethanolamine (tea) and metals General formula:

n[P(o-CH3)-C6H3-Och2Soo-·N+H(CH2CH2OH3]·MXm,

R=H, p-Cl, M=Mg, CA, Mn, Co, Ni, Cu, Zn, Rh, Ag; X=Cl, NO3CH3Soo;

n=1, 2; m=1-3, based on the reaction triethanolammonium salts o-resocialise or p-chloro-o-cratoxylon acids (trekrezan, KP and chlormezanone, XKP) of the above metals according to the scheme (1):

(I-XI)
I.R=HM=Zn,X=Cl,m=2,n=1.
II. R=HM=Zn,X=CH3Soo,m=2,n=1.
III.R=HM=Mn,X=Cl,m=2,n=2.
IV.R=HM=Ni,X=Cl,m=2,n=1.
V.R=HM-Co,X=Cl,m=2,n=1.
VI.R=HM=Ni,X=Cl,m=2,n=2.
VII.R=p-ClM=Rh,X=Cl,m=3,n=1.
VIII.R=HM=Ca,X-Clm=2,n=1.
IX.R=HM=Mg,X=Cl, m=2,n=1.
X.R=HM-AgX=NO3,m=1,n=2.
XI.R=HM-CuX=Cl,m=2,n=1.

According to x-ray diffraction [9] salts of triethanolamine (tricyclic have franowo structure (A), a closed three intramolecular trifurcation hydrogen bonds OH1and communication N→H, inward-looking protorennogo skeleton. They called us promatrani (PA), the structure of which is reflected by the formula:

where X=OOCH2OR.

Method of synthesis of PA was the reaction of the tea - N(CH2CH2OH)3with the appropriate acid. This way we first synthesized PA, which triethanolammonium salts of carboxylic acids, meets the General formula [10]:

RCH2COO-[NH(CH2CH2OH)3]+where R=H, o-CH3-C6H4O-CH3-p-Cl-C6H3O-CH3-C6H4S, p-Cl-C6H4S, p-Cl-C6H4SO2and other

It is obvious that the reaction of PA with metal salts n is the case reduce to the usual reaction of tea with salts of metals, which leads to the formation of known O-hydrometallation due to coordination BUT-M and N-M:

where M=metal; X=Cl, Br, I, NO3CH3Soo and others

Hydroxyl group and the nitrogen atom in the PA, through which the interaction with the metal atom (unlike the tea) is not free, and "connected" in atronomy skeleton (structure A). Therefore, to predict the course and in General the ability of the reaction cannot.

In the research we found that the reaction proceeds with formation of a ternary complex compounds as shown in scheme 1.

Reactions proceed with high yields (59-98%) of the target product in a solution of lower alcohols or water for 1-48 hours at room temperature. Three-component complex compounds emit distillation of the solvent, washing with ether and drying in a vacuum desiccator; they are powders of different colors (depending on the metal salt), soluble in water, alcohols, acetone, THF.

Thus, in the result of the research achieved the goal synthesized previously unknown type of the ternary complex compounds of metals with Tris(2-hydroxyethyl)ammonium salts of cresoxy - and p-chloro-o-resocialising acids and the way their gender is ing. The structure of the latter is proved by NMR(1H,13C), IR spectroscopy, elemental analysis data, as well as by potentiometric titration. The following examples illustrate the proposed method for three-component complex compounds.

Example 1. Synthesis of compound (I). CR·ZnCl2. To a solution of CU (0.66 g, 0.002 mol) in 10 ml of methanol was bury a methanol solution (10 ml) ZnCl2·1.5H2O (0.34 g, 0.002 mol). Was stirred at 25°for 12 hours. The solvent is kept in vacuum. The solid residue was repeatedly washed with ether, dried in a vacuum desiccator over P2O5. Received a colorless powder (yield 98%) with TPL 115°C, soluble in water and organic solvents (acetone, THF, alcohols). NMR1N (D2O): 7.05-6.62 (m,4H,C6H4O), 4.32 (s,2H,CH2Soo), 3.76 (s,6N,ON2), 3.28 (c,6H,3NCH2), 2.07(s,3H,C6H4-CH3). NMR13C(D2O): 176.99(C=O), 155.81 (C6H4O), 130.78-111.55 (C6H4), 66.89 (CH2MEO)55.09 (och2), 54.83 (NCH2), 15.28 (C6H4-CH3). IR: 1560(C=O), 3300 (OH).

Example 2. Synthesis of compound (II). CU·Zn(CH3Soo)2. Received likewise (I) from CU and zinc acetate (aspect]. 1:1) at 22°C in ethanol. Yield 89%. Colourless powder with TPL 103°C. NMR1H (acetone D6): 7.06-6.76 (m,4H,-C6H4O), 4.46 (s,2H,CH2Soo), 3.67(s,6N,ON 2), 2,78 (s,6N,3NCH2), 2.20 (s,3H,-C6H4-CH3), 1.88 (c,6H,2CH3COO). NMR13C (acetone D6): 177.00 (C=O), 156.56 -(C6H4O), 129.85-110.81, (C6H4), 78.00 (CH2MEO)57.12 (och2), 54.87 (NCH2),-At 28.27 (CH3MEO)15.22 (C6H4-CH3). IR: 1565 (C=O), 1620 (C=O), 3290 (HE).

Example 3. Synthesis of compound (III). 2KP·MnCl2. Received (I) from MnCl2·4H2O and CU (1:2) at 24-25°C for 24 hours. Yield 67%. Colourless powder with TPL 240°C. NMR1H(D2O): 6.83-6.52 (m,8H,2C6H4O), 3.53 (s,N,6OCH2), 3.05 (c,12H,6NCH2) 1.85 (s,6N,2C6H4-CH3). IR: 1584 (C=O), 3300 (OH). Found, %: C; N; N3.34; S; Mn 7.77. C30H50O12N2Mn. Calculated, %: C; N; N3.70; S; Mn7.27.

Example 4. The synthesis of the compound (IV). CR·NiCl2. Received likewise from CU and NiCl2·6H2O (1:1) in isopropyl alcohol. Yield 71%. Yellow powder with TPL 242°C (decomp.). NMR1H(D2O): 9.33-9.03 (m,4H,C6H4O), 6.06 (s,6N,3OCH2), 5.58 (c,6H,3NCH2), 4.40 (s,3H,C6H4-CH3). NMR13C(D2O): 178.91 (C=O), 157.00 (C6H4O), 124.12-114.80 (C6H4), 72.50 (CH2MEO)57.09 (och2), 56.84 (NCH2), 17.50 (C6H4-CH3). IR: 1590(C=O), 3300(OH). Found, %: C; N; N3.00; S; Ni 13.51. C15H25O6NCl2Ni. Calculated, %: C; N; N3.15; C115.94; Ni13.20.

Example 5. Synthesis Conn is in (V). CR·CoCl2. Received likewise (I) from CU and cobalt chloride when aspect]. 1:1 at room temperature. Yield 72%. Blue powder with TPL 240°C. IR: 1590(C=O), 3300 (OH).

Example 6. Synthesis of compound (VI). 2KP·NiCl2. Received (I) at 22°C for 48 hours. The reagent ratio 2:1. Yield 79%. Light green powder with TPL 180°C (decomp.). NMR1N (D2O): 7.06-6.68 (m,8H,2C6H4O), 3.79 (s,N,6OCH2), 3.31 (c,12H,6NCH2), 2.12 (s,6N,2C6H4-CH3). NMR13C(D2O): 178.17(C=O), 156.17 (C6H4O), 131.00-111.74 (C6H4), 69.90 (CH2Soo), 55.31 (OCH2), 55.02 (NCH2), 15.58 (C6H4-CH3). IR: 1605(C=O), 3160, 3310 (HE). Found, %: C47.36; N; N3.83; C19.21; Ni7.69. C30H50O12N2Cl2Ni. Calculated, %: C47.30; N; N3.68; C19.33; Ni7.62.

Example 7. Synthesis of compound (VII). HCR·RhCl3. Received likewise (I) of HCR and RhCl3·4H2O (1:1). Yield 70%. Red powder with TPL 160-165°C (decomp.). IR: 1590(C=O), 3300 (OH).

Example 8. Synthesis of compound (VIII). CR·CaCl2. Synthesized similarly to (I) of anhydrous calcium chloride and CU. Ratio (1:1). Yield 89%. Colourless powder with trasl. ≈250°C. NMR1H(D2O):7.08-6.65 (m,4H,2C6H4O), 4.34 (s,2H,CH2Soo), 3.80 (s,6N,6OCH2), 3.32 (c,6H,6NCH2), 2.10 (s,3H,2C6H4-CH3). NMR13C(D2O): 177.18(C=O), 156.08 (C6H4O), 131.03-111.61 (C6H4), 67.13 (CH2 Soo), 55.32 (OCH2), 55.03 (NCH2), 15.54 (C6H4-CH3). IR: 1585(C=O), 3310 (HE). Found, %: C at 42.85; N, 7.01; Cl 15.86; Sa 10.06. With15H25O6Nl2Sa. Calculated, %: 42.21; N, 5.90; Cl 16.60; Sa 10.56.

Example 9. The compound (IX). CR·MgCl2. Similarly, received from MgCl2·6H2O and CU. The output of 69.7%. Colourless powder with trasl. ≈230°C. NMR1N (D2O): 7.13-6.70 (m,4H,2C6H4O), 4.39 (s,2H,CH2Soo), 3.85 (s,6N,6OCH2), 3.25 (c,6H,6NCH2), 2.15 (s,3H,2C6H4-CH3). NMR13C(D2O): 177.16 (C=O), 156.08 (C6H4O), 131.04-111.61(C6H4), 67.09 (CH2Soo), 55.33 (och2), 55.04 (NCH2), 15.54 (C6H4-CH3). IR: 1610 (C=O), 3160, 3300(OH).

Example 10. Synthesis of compound (X). CR·AgNO3Received likewise (I) of AgNO3and CU (1:2) Output 69.44%. Pink powder with TPL 80°C. When stored in the light blackens. NMR1N (D2O): 7.09-6.68 (m,4H,2C6H4O), 4.34 (s,2H,CH2Soo), 3.79 (s,6N,6OCH2), 3.30 (c,6H,6NCH2), 2.11 (s,3H,2C6H4-CH3). NMR13With (D2O): 176.65 (C=O), 155.64 (C6H4O), 130.38-111,04 (C6H4), 66.59 (CH2COO), 54.88 (OCH2), 54.88 (NCH2), 15.04 (C6H4-CH3). IR: 1590 (C=O), 3320 (HE).

Example 11. Synthesis of compound (XI) CR·CuCl2. Synthesized similarly to (I) within 1 hour of CU and CuCl2·2H2O in water at 20°C. the Output 59.54%. Brown powder, do not have the s definite melting point. NMR1N (D2O): 7.10-6.60 (m,4H,2C6H40), 3.78 (s,6N,6OCH2), 3.31 (c,6H,6NCH2), 2.12 (s,3H,2C6H4-CH3). NMR13With (D2O): 177.85 (C=O), 154.74 (C6H4O), 132.10-110.00 (C6H4), 75.25.59 (CH2MEO)54.52 (och2), 54.52 (NCH2), 18.30 (C6H4-CH3). IR: 1610 (C=O), 3320 (HE).

Sources of information

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4. Voronkov M.G., Mirkova A.N., Levkovskaya, Dokl. An. 2002. T. S.

5. Voronkov M.G., Kolesnikova OP, M. Rasulov, Mirkova A.N. // Chem.-Pharm. W. 2007. V.5. S.

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1. A method of obtaining a three-component complex compounds o-cresoxy - and p-chloro-o-resocialising acid, triethanolamine and metals corresponding to the General formula:
n[R(o-CH )-C6H3-Och2Soo-·N+N(CH2CH2OH)3]·MXm,
where R=H, p-Cl, M=Mg, Ca, Mn, Co, Ni, Cu, Zn, Rh, Ag; X=Cl, NO3CH3Soo;
n=1, 2; m=1-3,
characterized in that triethanolammonium salt o-resocialising and p-chloro-o-resocialise acids interact with the corresponding metal salt in an alcohol or aqueous medium, preferably at room temperature for 1-48 hours

2. The method according to claim 1, characterized in that the separation of the ternary complex compounds carry out distillation of the solvent followed by washing the resulting powder with ether and drying in vacuum.



 

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16 cl, 3 tbl, 3 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a polyolefin synthesis method and more specifically to a polyethylene synthesis method. Polyethylene is a copolymer of ethylene with 1-alkenes. The invention also relates to polyethylene synthesis catalyst systems. The catalyst system is a mixture of metallocenes: hafnocene and an iron-based complex, an activating compound and a support. The invention also relates to films made from polyethylene and packets made from the said films.

EFFECT: disclosed catalyst system enables production of polyethylene with given molecular weight distribution in a single reactor.

16 cl, 3 tbl, 3 ex

FIELD: chemistry.

SUBSTANCE: method involves reaction in aqueous medium of a diaquaplatinum or bis(nitrato)platinum complex in a mixture with dihalogenoplatinum with a block-copolymer of formula (1): or (2):, where R1 represents hydrogen or C1-C12-alkyl, L1 and L2 - connecting groups, R3 - hydrogen, a protective group for amino groups, a hydrophobic or polymerised group, R4 represents hydroxy-, carboxy- or a hydrophobic group, R5 represents hydrogen, an alkali metal ion or a protective group for the carboxylic group, m=5-20000, n=10-60, under the condition that, R5 - hydrogen or an alkali metal ion constitutes 50% or more in n links.

EFFECT: obtaining a conjugate which does not contain silver ions, the solution of which has lower particle-size distribution.

17 cl, 11 dwg, 7 ex

FIELD: chemistry.

SUBSTANCE: invention relates to organometallic chemistry, specifically to a method of preparing a catalyst for metathesis polymerisation of dicyclopentadiene -[1,3-bis-(2,4,6-trimethylphenyl)-2-imidazolidinylidene]dichloro(o-N,N-dimethylaminomethylphenyl methylene)ruthenium. The method involves reacting a triphenylphosphine complex of ruthenium with 1,1-diphenyl-2-propin-1-ol in tetrahydrofuran while boiling in an inert atmosphere, and then with tricyclohexylphosphine at room temperature in an inert atmosphere. The indenylidene ruthenium complex formed is separated and successively reacted in a single reactor with 1,3-bis(2,4,6-trimethylphenyl)-2-trichloromethylimidazolidine and 2-(N,N-dimethylaminomethyl)styrene in toluene while heating in an inert atmosphere.

EFFECT: method increases output of product.

3 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing iron (II) oxalate by directly reacting metal with acid in the presence of atmospheric oxygen and a liquid phase while stirring. The process is carried out in a bead mill. The liquid phase solvent used is water with mass ratio of the liquid phase to glass beads equal to 1:1, content of oxalic acid in the initial load is between 0.5 and 2.0 mol/kg, and content of stimulating sodium chloride additive is between 0.02 and 0.10 mol/kg. Crushed grey cast iron which is stirred by a blade mixer is taken in amount of 30% of the mass of the rest of the load. The process is started and carried out at temperature in the interval from (50±2) to (93±2)°C while bubbling air under conditions for stabilising temperature using a heated liquid bath and controlling using a sample taking method and determination of content of iron (II) and (III) salts in the samples, and residual quantity of acid up to virtually complete conversion of the latter into salt. After that air bubbling, external heat supply for stabilising temperature and stirring are stopped. The suspension of the reaction mixture is separated from the glass beads and particles of unreacted metal alloy and filtered. The filtration residue is washed with distilled water and taken for further purification through recrystallisation, while the filtrate and the washing water are returned to the load for the repeated process. Iron (II) oxalate, which is separated from the reaction mixture by traditional filtering, is virtually the only product of conversion.

EFFECT: liquid phase used together with the sodium chloride additive can be repeatedly returned to the process.

10 ex, 1 tbl

FIELD: chemistry.

SUBSTANCE: catalysts for metathesis polymerisation of dicyclopentadiene are described, which are represented by [1,3-bis-(2,4,6-trimethylphenyl)-2-imidazolidinylidene]dichloro(o-N,N-diethylaminomethylphenylmethylene)ruthenium of formula (1) or [1,3-bis-(2,4,6-trimethylphenyl)-2-imidazolidinylidene]dichloro(o-N-pyrrolidinylmethylphenylmethylene)ruthenium of formula (2) . A method is described for producing a catalyst of formula (1), involving successively reacting a first generation Grubb catalyst with 1,3-bis-(2,4,6-trimethylphenyl)-2-trichloromethylimidazolidine and N,N-diethyl-(2-vinylbenzyl)amine in an inert atmosphere at temperature between 40 and 70°C in the presence of a solvent. In another version of the said method, a second generation Grubb catalyst is reacted with N,N-diethyl-(2-vinylbenzyl)amine in an inert atmosphere at temperature between 40 and 70°C in the presence of a solvent. A method is described for producing a catalyst of formula (2), involving successively reacting a first generation Grubb catalyst with 1,3-bis-(2,4,6-trimethylphenyl)-2-trichloromethylimidazolidine and 1-(2-vinylbenzyl)pyrrolidine in an inert atmosphere at temperature between 40 and 70°C in the presence of a solvent. In another version of the method, a second generation Grubb catalyst is reacted with 1-(2-vinylbenzyl)pyrrolidine in an inert atmosphere at temperature between 40 and 70°C in the presence of a solvent. A method is described for metathesis polymerisation of dicyclopentadiene, involving polymerisation using catalysts of formulae (1) or (2) in molar ratio monomer:catalyst ranging from 70000:1 to 100000:1.

EFFECT: increased output of catalyst and simpler synthesis due to less number of stages, obtaining polydicyclopentadiene with good application properties with low catalyst consumption.

7 cl, 6 ex

FIELD: chemistry.

SUBSTANCE: invention relates to method of producing manganese (II) alcoholates which can be used in different syntheses, in purification of complex multicomponent mixtures from alcohols, in analytical control and in scientific research. The method involves direct reaction of metal with alcohol in a vertical bead mill. The liquid phase used is the corresponding alcohol taken in mass ratio to glass beads of 1:1.5. Manganese is taken in amount of 5.81-43.3 % of the mass of the liquid phase. The process is initiated at room temperature and is carried out while controlling by taking samples and determination of content of manganese (II) compounds until all the loaded metal is virtually exhausted, after which stirring in the glass bead is stopped. The suspension of the reaction mixture is separated from the glass beads and taken for filtering. The alcoholate residue is washed with a liquid phase solvent and taken for purification by recrystallisation, and the filtrate and washing liquid phase with traces of dissolved alcoholate are returned for a repeated process. As a rule, the alcohol used is C1-C5-alcohol with normal and isomeric structure, cyclohexanol, ethyl cellosolve and ethylene glycol.

EFFECT: method allows for reaction of manganese with alcohol in conditions where the reaction could have been quantitatively insufficient with respect to the reagent, could have taken place at technically acceptable rates and led to accumulation the main mass of the product in solid phase, which can be easily separated by simple filtering.

2 cl, 2 tbl, 18 ex

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