Method of producing 1a-methyl-1a-(3'-thioalkylprop-2'-yl)-1ah-1(9)a-homo(c60-ih)[5,6]fullerenes |
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![Method of producing 1a-methyl-1a-(3'-thioalkylprop-2'-yl)-1ah-1(9)a-homo(c<sub>60</sub>-i<sub>h</sub>)[5,6]fullerenes](http://img.russianpatents.com/1116/11161650.gif)
IPC classes for russian patent Method of producing 1a-methyl-1a-(3'-thioalkylprop-2'-yl)-1ah-1(9)a-homo(c60-ih)[5,6]fullerenes (RU 2459805):
                
 Method for preparing trans-pinenyl sulfides / 2296749
Invention relates to chemistry of sulfur-containing organic compounds, namely, to a novel method of synthesis of trans-pinenyl sulfides of the general formula:
 Method for producing organic disulfides / 2091370
The invention relates to an improved process for the preparation of organic disulfides of the General formula R-S-S-R
 Method of producing dimethyl sulphide / 2457029
Invention relates to methods of producing sulphur-containing compounds, specifically dimethyl sulphide which is used as an odorant and starting material for synthesis of dimethyl sulphoxide which is used as a medicinal agent, solvent and extractant. Described is a method of producing dimethyl sulphide by converting dimethyl disulphide in the presence of methanol at atmospheric pressure and temperature 300-380°C using a catalyst containing gamma-aluminium oxide and 0.73-7.3 wt % chromium oxide. The weight ratio of methanol to dimethyl disulphide is equal to 0.8-0.9 g/g and contact time is 0.1-0.35 s.
 Prodrug 1,3-diamino-2-hydroxypropane derivatives / 2357962
Invention relates to the compounds of the formula
Method for modifying paraffins / 2313519
Invention relates to modification of oil paraffins, namely, to preparing sulfurous compounds used as additives in manufacturing bitumen in petroleum chemistry. Method involves interaction of paraffin with sulfur in the presence of alkaline metal persulfate or alkaline-earth metal persulfate, or ammonium persulfate. Invention provides preparing modified paraffins for a single step.
 The method of obtaining single-ended diallyldisulfide / 2223265
The invention relates to a method for producing an asymmetrical diallylsulfide General formula (1): R1-S-S-R2(1) where R1=CH3C2H5n-C4H9, R2=n-C6H13the h8H17the h9H19
 A method for production of alkyl - or alkylalkoxysilane / 2220134
The invention relates to a method for producing alkyl - or alkylalkoxysilane, which can serve as extractants of noble metals, flotation reagents, additives in oils, and can be used as starting compounds for the production of biologically active compounds, alkyl - or alkylalkoxysilane interaction of the corresponding mercaptan with alkyl - or alkenylphenol in the presence of an alkaline agent
 Composition based on dimethyl disulfide / 2219168
The invention relates to a composition based on dimethyl disulfide (DMDS)
 The method of obtaining serosoderjaschei additives / 2181137
The invention relates to the synthesis of serosoderjaschei additives with enhanced extreme-pressure, anti-wear properties, high thermal and oxidative stability
The method of obtaining serosoderjaschei additives / 2168536
The invention relates to the field of synthesis of serosoderjaschei additives with enhanced extreme-pressure, anti-wear properties, high thermal and oxidative stability
The method of obtaining polysulfide oligomers / 2154056
The invention relates to a process for the synthesis of polysulfide oligomers used as the basis sealant, adhesive and coating materials in various industries, including optical and optoelectronic engineering
 A method of producing dimethyl sulfide / 2032664
The invention relates to the chemistry of acyclic sulfides, specifically to an improved process for the preparation of dimethyl sulfide, which can be used as odorant and the source of raw material for the synthesis of dimethyl sulfoxide
 Method of producing 2-methylthioethanol / 2436770
Invention relates to production of thioethers from reaction of ethylene and organic thiols, and specifically to a method of producing 2-methylthioethanol, which is realised by reacting ethylene oxide with methyl mercaptan, with molar ratio of reagents equal to 1:1, in the presence of 10 wt % 2-methylthioethanol and is characterised by that the reaction takes place at temperature 30-40°C in the presence of a potassium hydroxide catalyst, taken in amount of 0.005-0.05 wt %, which is first dissolved in 2-methylthioethanol.
 Synthesis and use of 2-oxo-4-methylthiobutanoic acid, salts and derivatives thereof / 2385862
Invention relates to a method for synthesis of 2-oxo-methylthiobutanoic acid of formula (I) and its salts,
 Method of producing methionine / 2382768
Method involves the following steps: a) addition of at least one component selected from potassium carbonate, potassium bicarbonate or potassium hydroxide, to a solution containing 5-(β-methylmercaptoethyl)hydantoin for hydrolysis of 5-(β-methylmercaptoethyl)hydantoin to obtain a solution containing methionine; b) saturation of the solution containing methionine, carbon dioxide with precipitation methionine and separation of precipitated methionine together with separation of a first filtrate; c) division of the first filtrate into a first portion and a second portion, returning the first portion to step (a) and taking the second portion to step (d), where the first portion of the first filtrate may not be present; d) heating the second portion of the first filtrate to temperature above 200°C and pressure of water vapour formed during dwell time sufficient to obtain a filtrate heated to the required temperature, where the filtrate subjected to the said thermal treatment is directly saturated with carbon dioxide with precipitation of methionine and potassium bicarbonate, and the precipitated methionine and potassium bicarbonate are separated while also separating a second filtrate; and e) removal of the second filtrate or returning it to step a).
![Process of producing 2-amino-2[2-[4(3-benzyloxyphenylthio)-2-chlorophenylethyl]-1, 3-propanediol] hydrochloride and hydrates thereof, as well as intermediate products for producing said hydrates](http://img.russianpatents.com/img_data/1042/10420220-s.gif) Process of producing 2-amino-2[2-[4(3-benzyloxyphenylthio)-2-chlorophenylethyl]-1, 3-propanediol] hydrochloride and hydrates thereof, as well as intermediate products for producing said hydrates / 2376285
Invention relates to a method of producing 2-amino-2-[2-[4-(3-benzyloxy-phenylthio)-2-chlorophenyl]ethyl]-1,3-propanediol hydrochloride or its hydrate, involving the following steps: reacting 4-(3-benzyloxyphenylthio)-2-chlorobenzaldehyde and diethylphosphonoacetate ethyl in a solvent in the presence of a base, obtaining ethyl 3-[4-(3-benzyloxyphenylthio)-2-chlorophenyl]acrylate; reducing the formed ethyl 3-[4-(3-benzyloxyphenylthio)-2-chlorophenyl]acrylate with subsequent mesylation, iodizing, and nitration, obtaining 1-benzyloxy-3-[3-chloro-4-(3-nitropropyl-phenylthio]benzol; hydroxymethylation of the formed 1-benzyloxy-3-[3-chloro-4-(3-nitropropyl-phenylthio] benzol with formaldehyde, obtaining 2-[2-[4-(3-benzyloxyphenylthio)-2-chlorophenyl]ethyl]-2-nitro-1,3-propanediol; as well as reduction of the formed 2-[2-[4-(3-benzyloxyphenylthio)-2-chlorophenyl]ethyl]-2-nitro-1,3-propanediol, obtaining the end product. The invention also relates to intermediate products: ethyl 3-[4-(3-benzyloxyphenylthio)-2-chlorophenyl]acrylate, 1-benzyloxy-3-[3-chloro-4-(3-nitropropylphenylthio]benzol, 2-[2-[4-(3-benzyloxyphenylthio)-2-chlorophenyl]ethyl]-2-nitro-1,3-propanediol or to their hydrates.
Method of obtaining ammonium salt of 2-hydroxy-4-methylthiobutyric acid / 2355678
Invention concerns method of obtaining ammonium salt of 2-hydroxy-4-methylthiobutyric acid by reaction of 3-methylthiopropionic aldehyde with hydrogen cyanide, with obtainment of 2-hydroxy-4-methylthiobutyronitrile and further catalytic hydrolysis of indicated nitrile in the presence of titanium dioxide catalyst or its crystalline modifications. Anatase or anatase mix with rutile can be used as catalyst.
 Intermediate compounds useful in synthesis of hiv-protease inhibitors and methods for preparing these compounds / 2321580
Invention relates to a compound of the general formula: (R1)-(R2)-N-CH-(CH=CH2)-CH2R3 wherein R1 represents alkoxycarbonyl, arylalkoxycarbonyl, aryloxycarbonyl, benzoyloxycarbonyl; R2 represents hydrogen atom (H), or R1 and R2 in common with nitrogen atom to which they are joined form phthalimido, succinimido or N-diformyl group; R3 represents thioalkyl or thioaryl. Also, invention relates to a method for synthesis of compounds represented by the formula (8):
 Method for preparing methionine / 2294922
Invention describes a method of high volume density for synthesis of methionine. Method involves using a mixture comprising 3-methylmercaptopropionic aldehyde, hydrogen cyanide and carbon dioxide in the optional presence of water providing synthesis of 5-(2-methylmercaptoethyl)hydantoin and its conversion to methionine. Before passing carbon dioxide to a prepared mixture this aqueous mixture comprising compounds of the general formula: CnH2n+x-C=O-O-[CH2-CH2-O]m-H (1) wherein symbols have the following values: n means a whole number from 9 to 19; m means distribution in the range from 1 to 10; x means 1, -1, -3, -5 wherein 2n + x is 1, not less, and additive (2) as modified cellulose is added to hydrolysis solution prepared from 5-(2-methylmercaptoethyl)hydantoin in the mass ratio from 1:10 to 10:1 and in the total amount from 5 to 5000 ppm as measured for methionine in solution, and methionine is precipitated from solution followed by its dissolving and recrystallization. Invention provides reducing foam formation in synthesis of methionine, improved form of its crystals based on addition of carbon dioxide in precipitation of methionine from solution prepared as hydrolysis product. The additive (1) elicits anti-foaming effect while simultaneous presence of component (2) doesn't show negative effect on anti-foaming effect.
Method for preparing γ-ketosulfide concentrates / 2278110
Invention relates to a method for preparing concentrates of γ-ketosulfides. Method for preparing concentrates of γ-ketosulfides is based on the alkylthiomethylation reaction of ketones with a mixture of formaldehyde and methane gas odorant containing mercaptanes and disulfides in an aqueous-alkaline medium at temperature 20 ± 5°C. Proposed method provides enhancing the yield of the end product. Concentrates of γ-ketosulfides can be used as foaming agents-collecting agents in flotation of copper-zinc and gold-containing ores or adsorbents of sulfur dioxide.
 Method for preparing methionine / 2265593
Invention relates to a method for preparing methionine. Method involves: (a) hydrolysis of methionine amide in the presence of titanium-containing catalyst to obtain ammonium methioninate wherein indicated catalyst has bimodal distribution of pores and wherein indicated catalyst has distribution of pores size from at least 8 to 17 nm and distribution of pores sizes from 50 to 200 nm, the total volume of pores from 0.20 to 0.55 cm3/g and square surface from 30 to 150 m2/g, and (b) the second stage of regeneration of methionine from ammonium methioninate salt by removing ammonium. Also, invention claims industrial method for preparing methionine involving the abovementioned hydrolysis process. Method provides the complete conversion of methionine amide to methionine without additional treatment.
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FIELD: chemistry. SUBSTANCE: invention relates to organic chemistry, and specifically to a method of producing sulphur-containing homofullerenes of general formula (1): EFFECT: method of obtaining novel sulphur-containing homofullerenes, which can be used as effective nanocomponent additives for industrial oil, complexing agents, as well as novel optoelectronic materials. 1 cl, 1 tbl
The present invention relates to the field of organic synthesis, namely the method of production of 1A-methyl-1-(3'-toolkitpro-2'-yl)-1aH-1(9)a-Homo(C60-Ih)[5,6]fullerenes General formula (1):
R=Am (pencil), su (cyclohexyl). Sulfur-containing derivatives of fullerenes can be used as an effective nanocomponent additives for industrial oils, as well as new materials for optoelectronics (Usmjerili, Gnilichenko, Viglanoff, Agibalov, AirControl, Muds, And, Neropolis, Cal. RF patent №2382816 on 27.02.10 bull. No. 6 [1], A.Cravino, N.S.Sariciftci. J. Mater. Chem., 2Q02, 12, 1931 [2]). The known method (M.D.Meijer, B.Mulder, G.P.M. van Klink, G. van Koten. Inorganica Chimica Acta, 2003, 552, 247 [3]) obtain sulfur-containing methanofullerene (4) with the release of 24% response C60-fullerene (2) with the corresponding diazoketones (3), generated in situ by oxidation of hydrazone disubstituted benzaldehyde at room temperature for 96 h:
The known method does not allow to obtain 1a-methyl-1-(3'-toolkitpro-2'-yl)-an-1(9)a-Homo(C60-Ih)[5,6]fullerenes General formula (1). The known method (M.Prato, V.Lucchini, M.Maggini, E.Stimpfl, G.Scorrano, M.Eiermann, T.Suzuki, F.Wudl. J. Am. Chem. Soc., 1993, 115, 8479 [4]) get homoparental (6) and (7) in a mixture with meanfull the Wren (8) in the ratio 2:2:1 reaction of C 60-fullerene (3) phenyldiazonium (5) at room temperature
The known method does not allow to selectively receive 1A-methyl-1-(3'-toolkitpro-2'-yl)-1aH-1(9)a-Homo(C60-Ih)[5,6]fullerenes General formula (1). We propose a new method for selective receipt of 1A-methyl-1-(3'-toolkitpro-2'-yl)-1aH-1(9)a-Homo(C60-Ih)[5,6]fullerene (1). The method consists in the interaction of fullerene (C60with sulfur-containing diazoalkane generated in situ by oxidation of the corresponding hydrazones of ketosulfone using MPOs, the General formula N2C(Me)CH(Me)CH2S-R, where R=Am (pencil), su (cyclohexyl), in the presence of a three-component catalyst {Pd(acac)2:2PPh3:4Et3Al}, taken in a molar ratio of C60: vatsayana: Pd(acac)2: PPh3: Et3Al = 0.01:(0.01-0.03):(0.0015-0.0025):(0.003-0.005):(0.006-0.01), preferably 0.01:0.02:0.002:0.004:0.008, o-dichlorobenzene as a solvent at a temperature of 20°C for 0.25-1.0 hours Get 1A-methyl-1-(3'-toolkitpro-2'-yl)-1aH-1(9)a-Homo(C60-Ih)[5,6]fullerenes (1) with a total yield 36-60%. The reaction proceeds according to the scheme:
The conduct of a specified reaction in the presence of a palladium catalyst [Pd] more than 20 mol. % with respect to the fullerene C60does not lead to a significant increase in the yields of the target products (1). The use of palladium catalyst [Pd] in the amount of less than 20 mol. % with respect to the fullerene C60reduces the yield of the target product, which is associated with a decrease in reaction centers. The reaction should be carried out at room temperature (20°C). Carrying out the reaction at a higher temperature (e.g. 40°C) is associated with increased energy consumption. Significant differences of the proposed method: The proposed method is based on the generation of sulfur-containing diazoalkanes the in situ oxidation of hydrazones relevant metasulfite using MnO2and the use of catalytic quantities of palladium complex, the reaction is available in o-dichlorobenzene. The proposed method, in contrast to the known, allows you to selectively receive 1a-methyl-1-(3'-toolkitpro-2'-yl)-1aH-1(9)a-Homo(C60-Ih)[5,6]fullerenes (1), the synthesis of which are not described in literature. The method is illustrated by examples. To a solution of 0.002 mmol of Pd(acac)2in 0.5 ml of o-dichlorobenzene in a stream of dry argon at a temperature of -5°C and stirring 0.004 mmol PPh3, 0.008 mmol Et3Al and 0.01 mmol C60-fullerene in 1 ml of o-dichlorobenzene. To actionnow mass add 0.02 mmol hydrazone 3-(petitioner)-2-butanone in 0.2 ml of diethyl ether and portions 0.06 mmol MnO 2. After 0.5 h the reaction mass is diluted with 5 ml of toluene and passed through a column with a small layer of silica gel. Get 1A-methyl-1-(3'-tointerpret-2'-yl)-1aH-1(9)a-Homo(C60-Ih)[5,6]fullerene (1) with a total yield of 50% (according to HPLC). Spectral characteristics (1)
Other examples of the method are given in table 1
The reaction was carried out at room temperature in o-dichlorobenzene as a solvent. The method of obtaining 1A-methyl-1-(3'-toolkitpro-2'-yl)-1aH-1(9)a-d is(C 60-Ih)[5,6]fullerenes General formula (1):
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