Abstract:
A process for the preparation of 2,3,5-trimethyl-p-benzoquinone by oxidation of 2,3,5- or 2,3,6-trimethylphenol using oxygen or a gas mixture containing oxygen in the presence of a two-phase liquid reaction medium composed of water and a neocarboxylic acid having to 11 carbon atoms with a copper (II) halide-containing catalyst system at elevated temperature.
Abstract:
PROBLEM TO BE SOLVED: To provide an improved method for producing nicotinic acid, capable of profitably producing the nicotinic acid in a high yield by the direct oxidation of β-picoline by separately feeding the β-picoline and water into a reactor. SOLUTION: This method for producing nicotinic acid comprises separately feeding β-picoline and water into a reactor filled with a TiO2 support catalyst containing vanadium. This heterogeneous catalyst preferably contains anatase having a specific surface area of >100 m2/g as the support. The anatase support is preferably produced by a sulfate salt method. The titanium dioxide support preferably contains a sulfate salt in an amount of >0.1%. The catalyst preferably has a vanadium dioxide content of 5-50%. The reaction temperature is preferably 150-450 deg.C. The ratio of the acid/starting substance is preferably 5/1 to 40/1. The ratio of the water/starting substance is preferably 15/1 to 100/1. WHSV is preferably 0.02 to 5 h-1.
Abstract:
PROBLEM TO BE SOLVED: To produce the subject compounds in high yield by reacting a keto- isophorone with an acylating agent in the presence of a protonic acid and then saponifying the initially formed trimethylhydroquinone ester with an acid having a specific Hammett's constant. SOLUTION: (A) A 4-oxo-isophorone (keto-isophorone) represented by formula I is reacted with (B) an acylating agent (acetic anhydride, acetyl chloride, etc.), in the presence of a protonic acid and the initially formed trimethylhydroquinone ester is then saponified with an acid having
Abstract:
PROBLEM TO BE SOLVED: To provide an improved method for preparing α-tocopherol ester in a recycling method, wherein the reaction is made to proceed as far as possible in the direction of esterification in the first process, and the catalyst phase obtained in the reaction is regenerated after the finishing treatment by a method capable of readily recycling the catalyst to the reaction without lowering the catalyst activity. SOLUTION: A method for preparing α-tocopherol acetate in a recycling method comprises the following processes: trimethylhydroquinonediester is made to condense with isophytol in a mixture of a polar solvent, which is extractable with water or miscible with water, and water in the presence of a catalyst system containing zinc halide and an aqueous protonic acid, and optionally an elemental metal; and successively, the catalyst system is recycled.
Abstract:
PROBLEM TO BE SOLVED: To provide a method for producing 2,3,5-trimethylhydroquinone diester. SOLUTION: This method comprises producing 2,3,5-trimethylhydroquinone diester by aromatizing 2,6,6-trimethylcyclohex-2-ene-1,4-dione (4-oxo-isophorone, keto-isophorone, KIP) by using an acylating agent and an acidic soluble or insoluble catalyst. The method comprises (a) using a 1-4C alkyl group-containing carboxylic acid anhydride as an acylating agent, after the reaction, (b) distilling away a produced carboxylic acid, if necessary, (c) cooling a reaction solution, (d) separating a crystallized product and cleaning the product and (e) returning a filtrate to the process (a).
Abstract:
Process for the selective preparation of beta -isophorone epoxide by epoxidation of beta -isophorone with organic percarboxylic acids at a water content of less than 5 wt.%.
Abstract:
PROBLEM TO BE SOLVED: To provide a catalyst/solvent matrix needing no addition of an expensive new catalyst after condensation and capable of carrying out both the condensation and an after-acylation at medium temperatures. SOLUTION: A method for preparing α-tocopherol acetate in a recycling method comprises the following processes: trimethylhydroquinone is made to condense with isophytol in a mixture of a polar solvent, which is extractable with water or miscible with water, and water in the presence of a catalyst system consisting of zinc halide and an aqueous protonic acid, and optionally an elemental metal; successively, the resultant α-tocopherol is acylated; and the catalyst system is recycled.
Abstract:
PROBLEM TO BE SOLVED: To easily obtain a 2,3,5-trimethylhydroquinone diester useful as a synthetic intermediate for vitamin E, etc., in high yield by reacting a specific dione with an acylation agent in the presence of a specific easily handleable inexpensive catalyst. SOLUTION: The objective trimethylhydroquinone diester of formula II is produced by reacting 2,6,6-trimethyl-cyclohex-2-ene-1,4-dione of formula I (ketoisophorone or KIP) with an acylation agent in the presence of a catalytic amount of a protonic acid. The reaction is carried out by using an acid catalyst comprising one or more kinds of carboxylic acids (n) selected from orthoboric acid and/or boric anhydride or boric acid triester on one hand and from hydroxycarboxylic acid and a (hydroxy-containing) dicarboxylic acid or tricarboxylic acid on the other hand. The amount of the combined catalyst is preferably 0.1-10 mol%; based on the ketoisophorone used in the reaction.
Abstract:
PROBLEM TO BE SOLVED: To produce β-isophorone on an industrial scale at a low cost by isomerizing α-isophorone. SOLUTION: 3,5,5-Trimethylcyclohex-3-en-1-one(β-isophorone) is produced by isomerizing 3,5,5-trimethylcyclohex-2-en-1-one(α-isophorone) in liquid phase at 100-260 deg.C in the presence of a catalyst without adding other organic base. A salt-analog compound of the element of the group Ia or IIa of the periodic table or the element of the group Ia or IIa is used as the catalyst. The objective compound can be produced by a process simpler than conventional process and using smaller amount of catalyst with little production of by-product.
Abstract:
The reaction tube for preparing hydrogen cyanide comprises a cylindrical tube composed of ceramic, a catalyst comprising platinum applied to the inner wall of the tube and also at least one insert composed of ceramic, having three or four fins pointing from the tube axis to the inner wall of the tube, which is inserted into the cylindrical tube, wherein the fins divide the tube interior space into substantially straight channels with substantially identical circle segment cross sections and wherein the mean gap between the ends of the fins and the inner wall of the tube is in the range of 0.1 to 3 mm. In the method for preparing hydrogen cyanide, ammonia and at least one aliphatic hydrocarbon having 1 to 4 carbon atoms are reacted in the reaction tube at 1000 to 1400° C.