摘要:
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.
摘要:
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.
摘要:
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.
摘要:
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.
摘要:
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.
摘要:
The invention relates to a process for the preparation of methoxyacetic acid esters in which a chloroacetic acid ester is reacted with an alkali metal methoxide to give the methoxyacetic acid ester.
摘要:
The invention relates to a novel process for the simultaneous preparation of cyclopropyl alkyl ketones and 4,5-dihydroalkylfurans from 3-acyltetrahydrofuran-2-ones using a metal salt according to the diagram ##STR1## In the reaction, N-alkyllactams and/or N-acylmorpholines which are high-boiling and only slightly miscible with water are used. By charging the solvent, the metal salt and the 3-acyltetrahydrofuran-2-one in a molar excess with respect to the metal salt, heating the mixture to 160.degree. to 220.degree. C. and metering in further 3-acyl-tetrahydrofuran-2-one, the desired products are obtained in high yields. The metal salt can moreover be recovered in a simple manner by washing with water.
摘要:
In a process for the isolation of cobalt and/or manganese in the form of precipitated, easily filtrable cobalt and/or manganese oxalates from acetic acid solutions or extracts, the solutions in question are treated with oxalic acid dimethyl or diethyl ester at temperatures of 50.degree. to 250.degree. C.
摘要:
A process is provided for the recovery and recycling of spent cobalt and/or manganese catalysts used in the air oxidation of alkyl aromatics in acetic acid. The catalysts are isolated in the form of oxalates of extremely low solubility from the acetic acid mother liquors and the cobalt oxalate dihydrate and/or manganese oxalate dihydrate catalysts are restored by the joint action of hydrogen bromide and acetic anhydride, acetyl bromide, or a mixture thereof, to a form in which they are soluble in acetic acid and can be used, again, as oxidation catalysts.
摘要:
In a process for the recovery of cobalt oxalate and/or manganese oxalate, the solutions or extracts containing cobalt and/or manganese are treated with sodium, potassium or ammonium oxalate. To obtain an easily filtrable cobalt and/or manganese oxalate precipitate, the precipitation is performed at temperatures of 50.degree. to 160.degree. C. with 1 to 2 moles of solid alkali oxalate or ammonium oxalate. When sodium oxalate is used, the water content of the solutions or extracts is from 5 to 90% by weight, when potassium oxalate is used it is from 2 to 15% by weight, and when ammonium oxalate is used it is from 1 to 12% by weight.