The method of obtaining 4-cyclohexyl-4-methylpentene-2
(57) Abstract:The inventive product 4-cyclohexyl-4-methylpentane-2. Reagent 1: 4-phenyl-4-methyl-pentanone-2. Reagent 2: hydrogen. Reaction conditions: the hydrogenation is carried out in the presence of a copper-chromium catalyst at 210-250oand a pressure of 5.0-15.0 MPa, and the reaction mixture digitalout at 260-270oand a pressure of 0.2 to 2.5 MPa. table 2. The claimed method belongs to the technology of organic compounds, in particular the production of 4-cyclohexyl-4-methylpentene-2 (CIP) of the formula:
< / BR>CIP is used in perfumery and cosmetics industry as odorants.From analogs of well-known way to obtain DSM (the Netherlands, application N 300113 standard from 10.09.65) by hydrogenation of 4-phenyl-4-methylpentanol-2 over Raney Nickel at 150oC and 10.0 MPa, followed by oxidation of the obtained 4-cyclohexyl-4-methylpentanol-2 chromium mixture. This method has the following disadvantages:
the use of high-risk in the treatment of the catalyst;
the complexity of the technological design process associated with the filtration of fine catalyst;
a large amount of waste is diluted sulfuric acid containing toxic chromium salt;
required is a small autoclaves, the frequency of operation of the autoclaves.The closest analogue to the technical nature of the claimed is a method for CIP set forth in article journal "oil and Fat industry", 1958, No. 12, S. 23-25. "Catalytic dehydrogenation of alcohols", B. N. Karasev, A. A. Bach, L. L. Malkina, O. M. Holmer.The technical essence of the method according closest analogue is the dehydrogenation of 4-cyclohexyl-4-methylpentanol-2 in the presence of a copper-chromium catalyst supported on asbestos in the vapor phase. Synthesis is carried out by skipping pair of source materials through the catalyst at a residual pressure of 0.5 mm RT. Art. and temperature 240oC.This method has the following disadvantages:
low sensitivity of the original product;
little performance related to the process in the gas phase (less than 0.5 kg/l catches );
the complexity of the disposal of spent catalyst associated with use as a carrier of carcinogenic asbestos;
high energy costs and the complexity of the technological design associated using deep vacuum.The technical nature of the claimed method is that CIP was obtained as is at a temperature of 210-250oC and a pressure of 5.0-15.0 MPa, then the reaction mixture digitalout in a stream of nitrogen at a temperature of 260-275oC and a pressure of 0.2-2.5 MPa for copper-chromium catalyst.Stage hydrogenation according to the claimed method is performed at the following technological parameters:
the hydrogen pressure of 5.0-15.0 MPa
the temperature of the hydrogenation 210-250oC
contact load of 1.2-1.8 kg/l catches.Conversion at this stage is 90-95%
The second stage dehydrogenation is carried out at the following technological parameters:
a nitrogen pressure of 0.2-2.5 MPa
the temperature of the dehydrogenation 260-275oC
contact load 1.0 to 1.2 kg/l catches.Conversion of the target product is 90-95% Yield after CIP allocation is 82-90%
Control reaction mixtures is carried out by GLC.Stage hydrogenation and dehydrogenation is carried out in continuous mode, at a fixed-fixed catalysts.Below is a table 1 comparable data closest analogue and the claimed method.As you can see, the claimed method increases the yield of the target product and performance.Variant implementation of the claimed method # 1. oC at the same time serves 4-phenyl-4-methylpentane-2 with a speed of 18 ml/HR and hydrogen at a pressure of 10.0 MPa at a rate of 25 l/hThe reaction mixture containing 4-cyclohex - force-4-methylpentanol-2 is collected in the collection.The composition of the mixture, wt.4-Cyclohexyl-4-methylpentane-2 2,0
Volatile impurities 5,7
2. Into the reactor containing the recovered copper-chromium catalyst at a temperature of 260oC simultaneously serves obtained under item 1 of the reaction mixture at a rate of 12 ml/h and nitrogen at a pressure of 2.0 MPa at a rate of 25 l/hThe reaction mixture composition, wt.4-Cyclohexyl-4-methylpentane-2 95,0
Volatile impurities 1,7
3. The reaction mixture obtained under item 2, is subjected to vacuum distillation. Output 4-cyclohex-force-4-methylpentene-2 86%
4. The obtained 4-cyclohexyl-4-methylpentane-2 has the following physical specifications:
M. C. 182,30
d2409441 kg/m3< / BR>tKip239-240oC (75 mm RT.CT.)
Other options intervale, in table 2, including an implementation option # 1.As you can see, the claimed method provides a high yield of the product (see examples 1-3). Provided that the violation stated intervals (see examples 10-17 N) output is reduced.Based on the above description of the method of obtaining 4-cyclohexyl-4-methylpentene-2 inventive side claims that the specified object corresponds to a characteristic of the invention "industrial applicability" and is fully responsible for this criterion. The method of obtaining 4-cyclohexyl-4 methylpentene-2 using 4-cyclohexyl-4 methylpentanol-2, which digitalout in the presence of a copper-chromium catalyst at elevated temperature, characterized in that 4-phenyl-4-methylpentane-2 hydronaut in the presence of Nickel-copper-chromium catalyst at 210 250oC and a pressure of 5.0 15.0 MPa and the resulting reaction mixture containing 4-cyclohexyl-4-methylpentanol-2 digitalout in a stream of nitrogen at 260 270oC and a pressure of 0.2 to 2.5 MPa.
FIELD: organic chemistry, chemical technology.
SUBSTANCE: invention relates to a method for synthesis of 3-bromoadamantyl-1-alkyl(aryl)-ketones of the general formula: , wherein that can be used as intermediate substances for synthesis of some biologically active compounds. Method involves interaction of 1,3-dehydroadamantane with α-bromoketones of the following order: α-bromoacetone, α-bromoacetophenone, α-bromocyclohexanone in the mole ratio of reagents = 1:(2-3), respectively, in absolute diethyl ether medium, at temperature 34-40°C for 3-4 h. Method provides preparing the claimed compounds with high yield.
EFFECT: improved method of synthesis.
FIELD: industrial organic synthesis.
SUBSTANCE: invention relates to production of cyclohexanol or cyclohexanone via hydrogenation of phenol or benzene with hydrogen in presence of catalyst and diluent followed by hydration in case of using benzene as starting material. Process is characterized by that hydrogen and benzene or hydrogen and phenol preheated in heat exchanger, provided with condensate intake control circuit, and circulation gas are supplied to vaporizer and preheater, provided with heating steam consumption control circuits, through supply lines provided with shutoff valves. Phenol or benzene and circulation gas, as well as heating steam and condensate consumptions are specified and adjusted. Preheated mix is then fed into separator to separate gas from liquid phase, which is removed, while remaining gas mixture is sent to hydrogenation reactors comprising temperature control zones and heat-extracting tube-type condensers and provided with phenol or benzene, hydrogen and condensate control circuits, temperature sensors connected to controllers to adjust consumptions of phenol or benzene, hydrogen and condensate, and wherein diluent volume level compared to that of catalyst is controlled and hydration temperature is measured. Resulting product enters cooler and then separation column provided with cyclohexanol or cyclohexanone recovery level control and adjusting, wherefrom it is directed to gas circulation line comprising cooler, separator, and compressor equipped with pipelines with circulation gas consumption control circuits.
EFFECT: increased productivity with regard to cyclohexanol or cyclohexanone.
SUBSTANCE: invention concerns method of cyclic alkane oxidation by oxidation agent for obtaining a product, where oxidation is performed in cracking fractionator including vat zone at bottom end, head zone at top end, and reaction zone between vat and head zones. Reaction mix is kept boiling in reaction zone, and oxidation agent is added into reaction zone in at least two split flows. Non-reacted raw material leaving reaction zone is recycled into reaction zone. Gas containing molecular oxygen is used as oxidation agent, and reaction mix containing target product is collected below reaction zone.
EFFECT: simple and cost-effective method of obtaining the product, enhanced conversion of source material and selectivity of target product generation.
6 cl, 1 dwg, 3 ex
SUBSTANCE: claimed invention relates to a method of obtaining saturated aliphatic ketone, represented by the general formula (2), (where n stands for an integer number from 1 to 3; R represents a hydroxyl group, a cyclohexyl group, an alkyl group, which has from 1 to 4 carbon atoms, or an acyl group, which has from 1 to 4 carbon atoms), applied as an initial material for the production of medications, agrochemical preparations, optic functional materials and functional materials for electronics. The method consists in hydrogenation of a nucleus of an aromatic ketone, represented by the general formula (1), (where n stands for an integer number from 1 to 3; R represents a hydroxyl group, a phenyl group, an alkyl group, which has from 1 to 4 carbon atoms, or an acyl group, which has from 1 to 4 carbon atoms), with hydrogen under pressure in the presence of a solvent at a temperature from 20 to 120°C and in the presence of a catalyst, which carries from 0.1 to 20 wt % of the ruthenium atom on a carrier.
EFFECT: method makes it possible to obtain the target product with high selectivity.
6 cl, 24 ex
SUBSTANCE: method includes depositing an active component - copper - from an aqueous solution of an ammonia-carbonate complex on an oxide solid support, heat treatment and granulation. Deposition of the active component is carried out on an oxide solid support consisting of a mixture of white soot and boehmite in weight ratio of (2.5-3.5):1, and granulation of the catalyst paste is carried out by extrusion.
EFFECT: method enables to obtain a catalyst with high thermal stability while maintaining high selectivity and activity.
1 tbl, 4 ex
SUBSTANCE: method involves the preparation of cyclohexanone by cyclohexene oxidation, the isolation of cyclohexanone from a mixture of water-acetonitrile-cyclohexene-cyclohexanone of any composition by combining in the process scheme an autoclaving rectification with a medium-volatile separation agent acetonitrile and three-phase delamination in a Florentine vessel followed by feeding each layer to the rectification columns. The process scheme preferably comprises four distillation columns and a Florentine vessel.
EFFECT: separation of a reaction mixture of any composition into practically pure components that meet the quality requirements of marketable products.
2 cl, 2 dwg, 4 ex