Method of producing bis-semiquinolates of cobalt (ii), manganese (ii) and nickel (ii)

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing bis(3,6-di(tert-butyl)benzosemiquinolates-1,2) of cobalt (II) or manganese (II) or nickel (II), of general formula: M(SQ)2 , where: SQ is 3,6-di(tert-butyl)benzoquinolate-1,2, and M = Mn(II) or Co(II) or Ni(II). The method is characterised by that a disubstituted salt of an alkali metal salt and 3,6-di(tert-butyl) pyrocatechol-1,2 is obtained, followed by reaction thereof with 3,6-di(tert-butyl)benzoquinoline-1,2. The formed 3,6-di(tert-butyl)benzosemiquinolate-1,2 of the alkali metal reacts with a Co(II) or Mn(II) or Ni(II) halide in an inert atmosphere in tetrahydrofuran.

EFFECT: simple synthesis of bis-semiquinolates of metals.

4 cl, 5 ex

 

The invention relates to the production of spin-labeled bischelate metals of the first transition series, namely bis(3,6-di(tert-butyl)benzoimidazole-1,2) manganese(II), cobalt(II) and Nickel(II). The General formula of compounds, for which the claimed method of synthesis corresponds to M(SQ)2where SQ - 3,6-di(tert-butyl)benzoindole-1,2 and M=Mn(II) or Co(II), or Ni(II).

The structural formula of M(SQ)2below:

The compounds of this class can be used when creating heterospecific molecules with multiple paramagnetic centers, magnetoactive materials, namely photo - and thermoplasma spin switches, sensors near environment, the memory elements of the new type, as well as in organic synthesis.

Complexes of manganese(II) and Nickel(II) were previously synthesized by the reaction of CARBONYLS Mn2(CO)10and Ni(CO)4with 3,6-di(tert-butyl) - benzoquinone-1,2 in tetrahydrofuran (THF) under inert atmosphere (Inorg. Chem. 1998, 37, 3051; Izv. Acad. Of Sciences of the USSR, 1992, 2315, Inorg. Chem. 1992, 31, 3718). Compounds were extracted in the form of a solvate M(SQ)2(THF)2that was easily tsalala molecules of tetrahydrofuran THF during storage in air. A similar connection for cobalt to obtain by this method fails. Use in this reaction Co2(CO)8leads only to the formation of Tris[3,6-di(tert-butyl)benzo miminost-1,2]cobalt(III) (Co(SQ) 3) (Inorg. Chem. 1994, 33, 1276).

Used in the synthesis of the CARBONYLS of metals require special conditions when working with them, because they are volatile, toxic and can ignite upon contact with oxygen. In addition, they are unstable during storage and are quite expensive.

The invention solves the problem of creating a simple and economical method of obtaining bis(3,6-di(tert-butyl)benzoimidazole-1,2) cobalt(II) or manganese(II), or Nickel(II).

The proposed method of obtaining bis(3,6-di(tert-butyl)benzoimidazole-1,2) cobalt(II), manganese(II) and Nickel(II) lies in the interaction of halide Co(II), Mn(II) or Ni(II) with a solution of 3,6-di-tert-butylbenzothiazole-1,2 alkali metal in an inert atmosphere in tetrahydrofuran.

The proposed synthesis method was previously used to obtain Tris(3,5 - and 3,6-di(tert-butyl)benzoimidazole-1,2) transition metals III-VI group, and lanthanides (SU 527434, C07F 5/00, 05.09.1976).

It is proposed for use in obtaining bis(3,6-di(tert-butyl)benzoimidazole-1,2) transition metals VII-VIII groups. The method consists in the interaction of anhydrous halide Mn(II) or Co(II), or Ni(II) with a solution of 3,6-di(tert-butyl)benzoimidazole-1,2 alkali metal in tetrahydrofuran THF. The halide must be soluble in tetrahydrofuran THF, so for Mn(II) and Ni(II) possible use of bromide or iodide, and glaso(II) addition of bromide or iodide can also be used and chloride. The synthesis is carried out in an inert atmosphere at room temperature. This method allows to simplify the synthesis of the considered bis-semihydrate metals. In addition, it allows you to obtain the bis-chelate Co(SQ)2that it was not possible to allocate when using other synthesis methods.

The invention is illustrated by the following examples.

Example 1. Obtaining Co(SQ)2(THF)2.

All operations is carried out in an inert atmosphere. At room temperature 3,6-di(tert-butyl)benzoquinone-1,2 (Q) (0.50 g, 2.27 mmol) was dissolved in 15 ml of tetrahydrofuran (THF) and add an excess of metallic sodium. The mixture is stirred for ~5 h before formation of a light yellow solution of disubstituted salts of sodium and 3,6-di(tert-butyl)pyrocatechin-1,2. The resulting solution is filtered and added to it a solid Q (3,6-di(tert-butyl)benzoquinone-1,2) (0.50 g, 2.27 mmol). After dissolution of the added Q the solution becomes dark blue color is formed 3,6-di(tert-butyl)benzoimidazole-1,2 sodium. In the reaction mixture powder CoCl2(0.295 g, 2.27 mmol) and 25 ml THF. The mixture is stirred for 2 h, filtered and completely removed from the filtrate the solvent by a current of argon. The residue is treated with 15 ml F, the precipitate is filtered NaCl, added to the filtrate 35 ml of hexane and incubated the mixture at -18°C in a sealed flask for suto is. Formed small crystals of dark-blue color filtered off, washed with cold hexane, air-dried for 1 min (operations with segregated crystals can be performed in the air). Yield 78%.

Calculated for C36H56O6Co, %: C, 67.2; H, 8.8. Found, %: C, 67.0; H, 8.7.

For this complex is carried out x-ray analysis and identified the molecular and crystal structure.

Example 2. Obtaining Co(SQ)2(THF)2.

Similar to example 1. Differs in that it uses a powder of cobalt bromide CoBr2. Yield 71%.

Calculated for C36H56O6Co, %: C, 67.2; H, 8.8. Found, %: C, 67.1; H, 9.0.

Example 3. Obtain Ni(SQ)2(THF)2.

Ni(SQ)2(THF)2synthesized according to a similar method (example 1) of 0.50 g (2.27 mmol) NiBr2and 1 g (4.54 mmol) of 3,6-di(tert-butyl)benzoquinone-1,2. Yield 80%.

Calculated for C36H56O6Ni, %: C, 67.2; H, 8.8. Found, %: C, 66.9; H, 8.6.

Example 4. Obtain Ni(SQ)2(THF)2.

Similar to example 3. Characterized in that the alkali metal used potassium. Yield 74%.

Calculated for C36H56O6Ni, %: C, 67.2; H, 8.8. Found, %: C, 67.3, H 8.9.

Example 5. Obtain Mn(SQ)2(THF)2.

Mn(SQ)2(THF)2synthesized according to a similar method (example 1) of 0.50 g (2.27 mmol) MnBr2and 1 g (4.54 mmol) of 3,6-di(tert-butyl)benzoquinone-1,. Yield 67%.

Calculated for C36H56O6Mn, %: C, 67.6; H, 8.8. Found, %: C, 67.4; H, 8.7.

1. The method of obtaining bis(3,6-di(tert-butyl)benzoimidazole-1,2) cobalt(II)or manganese(II), or Nickel(II) General formula: M(SQ)2
,
where SQ - 3,6-di(tert-butyl)benzoindole-1,2 and M=Mn(II)or Co(II), or Ni(II), characterized in that the first stage receive duhsasana salt of an alkali metal and 3,6-di(tert-butyl)pyrocatechin-1,2, followed by its interaction with 3,6-di(tert-butyl) - benzoquinone-1,2 formed 3,6-di(tert-butyl)benzoimidazole-1,2 alkali metal is introduced into reaction with the halide(II)or Mn(II), or Ni(II) in an inert atmosphere in tetrahydrofuran.

2. The method according to claim 1, wherein the process is conducted at room temperature.

3. The method according to claim 1, characterized in that as halides Mn(II) or Ni(II) can be used bromide or iodide, and for Co(II) can also be used and chloride.

4. The method according to claim 1, characterized in that the alkali metal can be used sodium, potassium.



 

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14 cl, 35 ex, 4 tbl

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5 ex

FIELD: chemical technology.

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3 cl, 2 tbl, 21 ex

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5 dwg, 4 ex

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5 dwg, 4 ex

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25 cl, 17 ex, 23 tbl

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4 cl, 2 ex, 14 tbl

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2 cl, 11 ex

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2 cl, 2 tbl, 18 ex

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12 cl, 1 tbl, 3 dwg, 3 ex

FIELD: chemistry.

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2 cl, 11 ex

FIELD: chemistry.

SUBSTANCE: invention relates to an improved method of producing manganese (II) fumarate from manganese metal and its oxide (III) through direct reaction of the metal and its oxide Mn2O3 with an acid in the presence of a liquid phase and a stimulating iodine additive in a vertical type bead mill with glass beads as grinding agent. The metal and its oxide are loaded in molar ratio (2±0.1):1 in total amount of 7.87 to 10.93% of the mass of the load. Acid is added with 15 to 25% excess of the calculated value, equal to the number of moles of metal and twice the number of moles of metal oxide in the load. The base of the liquid phase is isoamyl alcohol, in which the iodine stimulating additive is dissolved in amount of 0.02 to 0.05 mol/kg. Glass beads are loaded first, in mass ratio to the reaction mixture of 1.35:1, and then later the liquid phase solvent, acid and stimulating additive, and after brief stirring, metal oxide and metal, stirring all the while. Taking this moment as the beginning of the process, forced cooling is introduced right away. Operating temperature is stabilised in the range 33 to 45°C and in this mode, the process is carried out until virtually quantitative conversion of metal and its oxide to the target salt, after which stirring and forced cooling are stopped. The reaction mixture is separated from the glass beads, cooled to temperature 5 to 6°C and kept at that temperature for 1 to 2 hours. The solid phase of the target salt is filtered off and washed with isoamyl on a filter cooled to approximately the same temperature, after which it is taken for purification by recrystallisation. The filtrate and the cleaning solvent, containing excess acid, the bulk of the stimulating additive and a certain amount of dissolved target salt, are returned for loading in the repeated process. The process is carried out in light temperature conditions. The target substance can be easily separated.

EFFECT: design of a low-waste method, which allows for obtaining target product from available manganese oxide with an easy to implement process.

9 ex

FIELD: medicine.

SUBSTANCE: invention refers to chelating agents and their technetium complexes to be used as radiopharmaceuticals and characterised by formula I where X is -NR-, -CO2-, -CO-, -NR(C=S)-, -NR(C=O)-, -CONR- or Q; Y represents amino acid, -CH2-, -CH2OCH2-, -OCH2CH2O- or X; Z is an aggregation from peptides, their analogues, substrata, antagonists or enzyme inhibitors, receptor-bonding compounds, oligonucleotides, oligo-DNA- or oligo-RNA-fragments; n is a number 1 to 8; m is a number 0 to 30; R represents H, C1-4alkyl, C2-4alkoxyalkyl, C1-4hydroxyalkyl or C1-4fluoroalkyl; Q represents remains of succinimide , A is a pharmaceutically acceptable anion.

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22 cl, 12 ex, 3 dwg, 2 tbl

FIELD: chemistry.

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EFFECT: method makes it possible to produce target product in absence of manganese dioxide and stimulating additive at temperatures close to room temperature.

2 cl, 13 ex, 2 tbl

FIELD: chemical industry; methods of production of the manganese salts with the organic acids.

SUBSTANCE: the invention is pertaining to production of the manganese salts with the organic acids in particular, to the salt of the divalent manganese and formic acid. The method is exercised by interaction of manganese, its oxides in the state of the highest valence with the formic acid solution in the organic solvent in the presence of iodine as the stimulating additive. The production process is conducted in the bead grinder of the vertical type having the revertive cooler-condenser, the high-speed paddle stirrer and the glass beads of in the capacity of the grinding agent loaded in the mass ratio to the loading of the liquid phase as (1÷2): 1. The liquid phase consists of the formic acid solution in the organic solvent. The concentration of the acid is taken within the range of 3.5÷10.8 mole/kg. In the loaded liquid phase they dissolve the stimulating additive of iodine in the amount of 0.025-0.100 mole/kg of the liquid phase. The ratio of the masses of the liquid phase and the total of the metallic manganese and the manganese oxide are as(4.9÷11):1. The molar ratio of the metal and the oxide in the loading is as (1.8÷2.,2):1. The metal and the oxide are loaded the last. It is preferable in the capacity of the dissolvent to use the butyl alcohol, ethyl acetate, ethylene glycol, 1.4-dioxane, dimethyl formamide. The production process is started and conducted at the indoor temperature up to practically complete(consumption of the whole loaded manganese oxide. Then the stirring is stopped, the suspension of the salt is separated from the beads and the nonreacted manganese and after that conduct filtration. The filtrate and the nonreacted manganese are returned into the repeated production process, and the filtered out settling of the manganese salt is exposed to purification by recrystallization. The technical result of the invention is - simplification of the method at usage of accessible reactants.

EFFECT: the invention ensures simplification of the method at usage of accessible reactants.

16 ex, 2 tbl

FIELD: process engineering.

SUBSTANCE: invention relates to petrochemical and chemical industries, particularly, to production of methane conversion catalyst, method of its production and method of converting methane into aromatic hydrocarbons in nonoxidising conditions. Zeolite catalyst comprises molybdenum in amount of not over 4.0 % by wt as modifying element, carbamide as structure-forming additive, and nano-sized silver powder as second modifying element, said silver powder produced by conductor electrical blasting, at concentration varying from 0.1 to 2.0 wt %. Proposed method allows producing catalyst by dry mixing of zeolite modified by molybdenum with molybdenum content not exceeding 4.0 wt % with second promoting agent, i.e. nano-sized silver powder with its content in produced catalyst varying from 0.1 to 2.0 wt %. Method of methane nonoxidising conversion is performed in the presence of above described catalyst.

EFFECT: higher degree of methane conversion and yield of aromatic hydrocarbons along with catalyst longer life.

3 cl, 1 tbl, 8 ex

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