Abstract:
(2RS,3RS)-3-(2'-aminophenylthio)-2-hydroxy-3-(4"-methoxyphenyl)-propionic acid methyl ester, an important precursor for the preparation of the pharmaceutical active substance diltiazem, is obtained in a particularly high stereoselectivity and yield by addition of o-aminothiophenol onto 3-(4'-methoxyphenyl)-glycidic acid methyl ester if the reaction is carried out in the presence of alkali metal salts of weak acids in the presence of catalytic amounts of iron compounds.
Abstract:
2-Chloroacrylonitrile is prepared in a particularly advantageous and readily industrially practicable manner by chlorinating acrylonitrile and then thermally cleaving the 2,3-diehloropropionitrile formed, by chlorinating acrylonitrile in the presence of a catalyst system comprising dimethylformamide and pyridine and/or pyridine derivatives and subjecting the resulting crude 2,3-dichloropropionitrile to thermal cleavage in the presence of the same catalyst system without the addition of further catalysts.
Abstract:
4-Fluorothiophenol is obtained in outstanding purifies and yields if 4-fluorobenzenesulphonyl chloride is reacted with sodium hydrogen sulphite solution to give a solution of sodium 4-fluorobenzenesulphinate, this solution is reduced with sulphur dioxide to give 4,4'-difluorodiphenyl disulphide and finally this is reacted with sodium borohydride in a water-miscible inert organic solvent to give 4-fluorothiophenol (sodium salt). Free 4-fluorothiophenol can be isolated from the sodium salt solution by acidification.
Abstract:
2-(Arylimino-methyl)-3-dialkylaminoacrylonitriles can be obtained by reaction of .beta.-anilino-acrylonitriles with ortho-formamides. They are suitable as starting substances for the preparation of 4-amino-5-iminiummethylene-2-pyrimidines or 4-amino-5-formyl-2-pyrimidines.
Abstract:
Dialkyl dicarbonates are obtained particularly advantageously from halogenoformic esters by reaction with alkalis in the presence of water-immiscible organic solvents and in the presence of a catalyst, if the catalyst used is benzylalkyldimethylammonium halides. The catalyst is then particularly easy to separate off and to recycle from the reaction mixture.
Abstract:
Mixtures consisting essentially of cyclohexylbiphenyls, dicyclohexylbenzenes, phenylbicyclohexyls and tercyclohexyls are outstandingly suitable as heat transfer media. The mixtures can be prepared from biphenyl and cyclohexanol in the presence of bleaching earths and subsequent hydrogenation.
Abstract:
The halogen of a polyhalogenated aromatic compound can be transferred to a monohalogenated or nonhalogenated aromatic compound by reaction in the presence of ruthenium as the element or in the form of compounds and if desired with one or more metal compounds from subgroups I and II of the Periodic Table.
Abstract:
Aromatic hydrocarbons monosubstituted by straight-chain or branched C.sub.1 -C.sub.12 -alkyl or by Chd 3-C.sub.8 -cycloalkyl can be chlorinated in the aromatic ring in the liquid phase in the presence of Friedel-Crafts catalysts if cyclic amidines which are oxy-sustituted on the exocyclic N atom are employed as co-catalysts. An increased proportion of the p-isomer is obtained in this reaction.
Abstract:
4,4-Dimethyl-1-(p-chlorophenyl)pentan-3-one can be prepared by condensation of pinacolone and p-chlorobenzaldehyde in an alcohol as solvent in the presence of an inorganic base and by subsequent hydrogenation, in which the reaction mixture obtained in the condensation is hydrogenated directly without isolation of the intermediate 4,4-dimethyl-1-(p-chlorophenyl)-1-penten-3-one after the addition of a hydrogenation catalyst at elevated temperature and superatmospheric pressure to give 4,4-dimethyl-1-(p-chlorophenyl)pentan-3-one, after the hydrogenation catalyst has been separated off from the liquid hydrogenation mixture, the alcohol is largely distilled off, and the water content of the bottom product of the distillation is adjusted in such a manner that it separates into an aqueous and an organic phase, and the 4,4-dimethyl-1-(p-chlorophenyl)pentan-3-one is recovered from the organic phase.
Abstract:
Aromatic hydrocarbons which are monosubstituted by straight-chain or branched C.sub.1 -C.sub.12 -alkyl or by C.sub.3 -C.sub.8 -cycloalkyl can be chlorinated in the presence of Friedel-Crafts Catalysts in liquid phase on the aromatic ring if 1,6-benzothiazocins are used as co-catalysts. This makes it possible to obtain a higher proportion of p-isomers.