摘要:
An improved process for the preparation of pivaloylacetic acid esters by decarbonylation of pivaloylpyruvic acid esters at elevated temperatures is described. The process is carried out in the presence of 0.01 to 5 percent by weight of a metal of sub-groups one to eight of the periodic system, which metal is in metallic and/or oxidic form. Initially, 30 percent of the pivaloylpyruvic acid ester to be converted is heated in the presence of the metal, and after conversion of the same there is added additional pivaloylpyruvic acid ester according to the rate at which the pivaloylpyruvic acid ester is converted.
摘要:
Aromatic aminosulphonic acids which have a reduced content of discoloring by-products are obtained when aromatic amines are reacted with a sulphonating agent in a reaction medium at least some of which consists of tetramethylene sulphone.
摘要:
Aminoarylsulphonic acids which have a relatively high purity and a relatively low content of aminoaryldisulphonic acids can be obtained, if they are prepared, from the corresponding arylammonium hydrogen sulphates, by an improved version of the so-called baking process, wherein the reaction is carried out under pressure at a temperature of at least 140.degree. C. and, at least partially, in the presence of water.
摘要:
The invention relates to a process for isolating H acid and K acid in the form of their monoalkali metal salts from acid aqueous solutions which contain these two acids and alkali metal ions and may contain other aminonaphtholdisulphonic acids, in which process H acid monoalkali metal salts are precipitated at elevated temperatures from solutions which contain not only sodium ions but also potassium ions and then precipitating K acid monoalkali metal salts by cooling down the filtrate obtained after separating off the H acid monoalkali metal salts.
摘要:
In the preparation of 4-amino-6-tert.-butyl-3-methylthio-1,2,4-triazin-5-(4H)-one of the formula ##STR1## wherein pivaloyl cyanide of the formula(CH.sub.3).sub.3 C--CO--CNis reacted to form an intermediate, the intermediate is condensed with thiocarbohydrazide of the formulaNH.sub.2 --NH--CS--NH--NH.sub.2to form 4-amino-6-tert.-butyl-3-mercapto-1,2,4-triazin-5-(4H)-one of the formula ##STR2## and the 4-amino-6-tert.-butyl-3-mercapto-1,2,4-triazin-5-(4H)-one is alkylated to replace the H atom on the sulphur by --C.sub.1-4 --alkyl, the improvement which comprises reacting the pivaloyl cyanide with a carboxylic acid anhydride of the formulaR--CO--O--CO--Rin which R is an optionally substituted aliphatic radical with up to 8 carbon atoms or an optionally substituted phenyl radical, in the presence of a strong acid at a temperature between about -50.degree. and +150.degree. C., and then directly reacting the reaction mixture thus obtained with the thiocarbahydrazide. Advantageously R is CH.sub.3, the strong acid is concentrated sulphuric acid, the pivaloyl cyanide is effected at a temperature between about 0.degree. and 100.degree. C., the condensation with thiocarbohydrazide is effected, in the presence of a mineral acid, in an aqueous or aqueous-alcoholic medium, and the alkylation is effected using methyl iodide or methyl bromide in the presence of sodium hydroxide at about 0.degree. to 50.degree. C.
摘要:
The present invention relates to dichloromaleic acid diamides of the formula ##STR1## in which R represents an optionally substituted aliphatic radical with up to 8 carbon atoms, a cycloalkyl radical with 3 to 6 carbon atoms or a substituted phenyl radical which possess fungicidal properties and are produced by reacting a dichloromaleic acid halide of the formula ##STR2## in which X is halogen with an amine of the formulaH.sub.2 N--Rin a diluent and in the presence of an acid-binding agent.
摘要:
A process for the preparation of a sulfonic acid chloride of the formula ##STR1## wherein R.sup.1, R.sup.2 and R.sup.3 are identical or different and denote hydrogen, a lower alkyl or cycloalkyl radical, halogen, aryl, aralkyl, aryl-ether or one of the radicals ##STR2## or where ADJACENT RADICALS R.sup.1 and R.sup.2 are linked to form a cycloaliphatic or aromatic carbocyclic ring which is optionally substituted by a sulfonic acid chloride groupWhich comprises contacting an aromatic compound of the formula ##STR3## wherein R.sup.1, R.sup.2 and R.sup.3 have the previously assigned significanceWith an approximately equimolar amount of a sulfonating agent, based upon the number of sulfonic acid chloride groups to be introduced and an excess of thionyl chloride, the sulfonating agent and thionyl chloride being initially introduced or added simultaneously with the addition of said aromatic compound.
摘要:
Cyclopropanecarboxamide can be prepared by reaction of a cyclopropanecarboxylic ester with NH.sub.3, in which the ester alcohol has 4-8 C atoms and can be straight-chain or branched and which process is carried out in the presence of catalytic amounts of an alkali metal alcoholate of a monohydric C.sub.1-C.sub.8 alcohol at 60.degree.-200.degree. C. in the absence of a hydrocarbon solvent.
摘要:
The characteristic of the improved process for the preparation of 1,5-dihydroxynaphthalene and 1,5-diaminonaphthalene is to carry out the alkaline pressure hydrolysis of the disodium salt of naphthalene-1,5-disulphonic acid at temperatures from 270.degree. to 290.degree. C. and under 14 to 20 bar using an excess of sodium hydroxide solution such that the molar ratio NaOH/disodium salt of naphthalenesulphonic acid is at least 12:1. The 1,5-dihydroxynaphthalene which is obtained in this manner, without hazard and in substantially higher purity, is then aminated with ammonia in the presence of ammonium bisulphite to give 1,5-diaminonaphthalene, it being possible to achieve a further increase in the degree of purity of the 1,5-diaminonaphthalene by increasing the molar ratio NH.sub.3 /1,5-dihydroxynaphthalene to at least 6:1.
摘要:
New process for the preparation of 1-aminonaphthalene-2,4,7-trisulphonic acid and, if appropriate, 1,7-Cleve's acid, in which 1-nitronaphthalene is reacted by the Piria method with bisulphites in a manner which is known per se, the sulphamate mixture obtained in this Piria reaction is sulphonated with sulphur trioxide in sulphuric acid to give 1-aminonaphthalene-2,4,7-trisulphonic acid and, if appropriate, this is hydrolysed to 1,7-Cleve's acid by heating in aqueous sulphuric acid.