Abstract:
The invention relates to a process for the preparation of a macrocyclic ester of the general formula: in which m is an integer from 6 to 14 and n is an integer from 2 to 12.
Abstract:
Cyclopropylamine is prepared from butyrolactone by a process comprising:(a) reacting butyrolactone with hydrogen chloride, thereby yielding chlorobutyric acid, (b) esterifying said chlorobutyric acid with a primary or secondary alcohol having 4-8 carbon atoms, (c) cyclizing the ester with an alkali metal alcoholate of a primary alcohol having 1-3 carbon atoms to give a mixture of cyclopropanecarboxylic acid esters, (d) converting the cyclopropanecarboxylic acid ester mixture into cyclopropanecarboxylic acid amide by reacting the ester mixture with ammonia, and (e) reacting said cyclopropanecarboxylic acid amide with hypohalite ion in a basic medium, thereby forming cyclopropylamine.
Abstract:
The invention relates to a process for the preparation of aminomalonic acid esters and optionally their salts by the catalytic hydrogenation of a substituted malonic acid ester in an inert solvent, and optionally by the addition of an acid to the hydrogenation mixture. The process comprises carrying out the hydrogenation in the presence of a solid dehydrating agent and a solvent or solvent mixture in which the aminomalonic acid ester salt is substantially insoluble.
Abstract:
For the preparation of 2-cyanoacetoxypropionic esters, a mixture of lactic ester and cyanoacetic ester is introduced, an alkali metal alcoholate is added as catalyst and the mixture is heated while the alcohol eliminated during the course of the reaction is distilled off. The course of the reaction is followed by means of gas chromatographic analysis and the reaction is terminated prior to eliminating the theoretical amount of alcohol by destroying the catalyst by acidification. The reaction mixture is worked up by distillation and the product easily separated from the reaction mass due to the substantial absence of high boiling components.
Abstract:
In a process for preparing aromatic monocarboxylic acids by oxidation of toluene or of toluenes substituted in the nucleus, the starting substances are reacted in the liquid phase with oxygen or with a gas containing oxygen, at a temperature of 80.degree.-180.degree. C. and a pressure of 5 to 50 bar in the presence of acetic acid as diluent and a soluble cobalt and/or manganese salt in combination with a bromide, and the aromatic monocarboxylic acids are then obtained by solid-liquid separation of the cooled reaction mixture.To reduce the dimensions of the oxidation reactor, for which particularly corrosion-resistant materials are necessary, and to isolate the target products in high yield and purity, as well as to reduce the technical complexity and cost of the treatment of the amounts of solvents that are yielded, relatively small amounts of acetic acid are used as solvents or diluents, namely at a ratio by weight of the alkyl aromatic being oxidized and acetic acid of 0.5:1 to 6:1. Not until the reaction has ended is the dilution, which is necessary for the isolation of the target product by solid-liquid separation of the cooled reaction mixture, performed by the addition of dilute aqueous acetic acid or of the washing filtrate from a preceding oxidation run. A typical example is the preparation of p-tert-butylbenzoic acid from p-tert-butyltoluene by the method described.
Abstract:
A process for preparing potassium monoethyl malonate by selective saponification of malonic acid diethyl ester with potassium hydroxide, in which the potassium hydroxide is added to the malonic acid diethyl ester, malonic acid diethyl ester and potassium hydroxide are used in a molar ratio of at least 1.5 and the potassium hydroxide is effectively distributed into the malonic acid diethyl ester.
Abstract:
A three-stage process for removing mercury contaminants from alcoholic alkali metal alkoxide solutions is provided, in which mercury is depleted in a first filtration through inert fibrous material, followed by a second filtration through pulverized coal, and then by concentration by distillation, to preferably provide a mercury content below 0.1 ppm.
Abstract:
Alkali metal salts of cyanoacetone are prepared by reacting an acetonitrile, an acetic acid ester and an alkali metal alkoxide without distilling off the alcohol formed during the reaction. The reaction products are obtained with high yields and high purity.
Abstract:
2-(methylthio)barbituric acid is obtained with high yields and degree of purity by reacting a solution or suspension of an alkali metal salt or alkaline earth metal salt of 2-thiobarbituric acid with methyl bromide at a pressure of 1.5 to 5 bar.
Abstract:
The invention relates to enantiomerically enriched malonic acid monoesters &agr;-monosubstituted by a tertiary hydrocarbon radical, or their salts, of the general formula I: in which R1, R3, R4 and R5 are identical or different hydrocarbon radicals, and wherein any two of the radicals R3, R4 and R5 may alternatively be present as a carbocyclic ring together with the quaternary carbon atom which they substitute, and M is hydrogen, one equivalent of a metal or an optionally substituted ammonium ion. The invention further relates to a process for the preparation of the enantiomerically enriched &agr;-monosubstituted malonic acid monoesters, or their salts, by enzymatic partial hydrolysis of the corresponding diesters.