摘要:
A process has been invented for the preparation of naphthalene-1,3,6-trisulphonic acid by sulphonating naphthalene with sulphuric acid and oleum, characterized in that naphthalene and most of the oleum are simultaneously metered into sulphuric acid or oleum of low concentration, which has been initially introduced, at about 140.degree. to 240.degree. C., the temperature is kept at about 140.degree. to 240.degree. C. for some time, the remainder of the oleum is then added at about 140.degree. to 240.degree. C. and the mixture is then further stirred for some time.Naphthalene-1,3,6-trisulphonic acid is a known important intermediate used, for example, in the preparation of T-acid, H-acid and chromotropic acid.
摘要:
A process for producing the magnesium salt of 3-nitro-naphthalene-1,5-disulfonic acid by sulfonating naphthalene, nitrating the sulfonation product, and separating the pure magnesium salt of 3-nitronaphthalene-1,5-disulfonic acid, which process comprises:(a) sulfonating naphthalene with liquid SO.sub.3 in the presence of an inert organic solvent at temperatures between -40.degree. and +20.degree. C.;(b) adding to the reaction mixture obtained a mixture consisting of about equal parts of 100% sulfuric acid and fully reacted crude nitration mixture from nitration of a previous nitration charge, separating from the resulting two-phase system the upper organic solvent phase by decanting, and removing from the Armstrong's acid anhydride acid slurry the remainder of organic solvent by distillation, or removing it during or after subsequent nitration, subsequently adding to the residue the amount of nitric acid required for nitration, and then nitrating;(c) adding then firstly water and afterwards, in the absence of the inert organic solvent, at 90.degree. to 120.degree. C., a compound releasing magnesium ions, the amount being such that, per mol of 3-nitronaphthalene-1,5-disulfonic acid, 1.1 to 1.3 mols of magnesium ions are added, and a sulfuric acid concentration of between 40 and 60 percent by weight (relative to the sulfuric acid and water) is maintained; and(d) separating the crystallized magnesium salt of 3-nitronaphthalene-1,5-disulfonic acid at a temperature of between 20.degree. and 70.degree. C., and subsequently optionally washing it with a maximum of 60 percent by weight of sulfuric acid and/or water, and optionally drying the product.
摘要:
A process has been invented for the preparation of aminonaphthalenesulphonic acids by the catalytic hydrogenation of salts of nitronaphthalenesulphonic acids with hydrogen in the presence of Raney nickel catalysts at elevated temperature and pressure, said catalysts comprising a combination of fresh Raney nickel catalyst and Raney nickel catalyst which has already been used in prior hydrogenation or hydrogenations.
摘要:
2-Amino-5-alkyl-phenols, which are suitable as intermediates in the production of crop-protection agents or photographic couplers, can be prepared by subjecting 2-amino-5-alkyl-benzenesulphonic acids or their salts to alkaline hydrolysis.
摘要:
The invention relates to a process for the preparation of 1-amino-8-naphthol-3,6-disulphonic acid (H-acid) as the mono-alkali metal salt from napthylamine-trisulphonic acid isomer mixtures by alkaline hydrolysis under pressure. The separation of the H-acid is effected by utilizing an aqueous sulphuric acid which contains naphthalene- and/or nitronaphthalene- and/or naphthylamine- and/or naphthol- and/or aminonaphthol-mono-, -di-and/or-tri-sulphonic acids.
摘要:
The invention relates to a method for the preparation of 4,6-dichloropyrimidine by reacting 4-chloro-6-methoxypyrimidine with at least one sulphur-containing chlorinating agent selected from the group consisting of SCl2, SOCl2, and SO2Cl2 in the presence of at least one phosphorus compound having the formula R3P═Yn (1), in which R represents C1-C10-alkyl or C6-C10-aryl, each of which may optionally be substituted by up to five identical or different substituents selected from the group consisting of fluorine, chlorine, bromine, C1-C4-alkyl, and C1-C4-alkoxy, Y represents oxygen or sulphur, and n represents zero or 1.
摘要:
The invention relates to a process for the preparation of 4,5,6-trichloro- and 2,4,5,6-tetrachloropyrimidine starting from 3-dimethylamino-propionitrile, to its use and also to a crystalline intermediate product form.
摘要:
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.
摘要:
The invention relates to a method for the preparation of 4,6-dichloropyrimidine by reacting 4-chloro-6-methoxypyrimidine with phosgene as chlorinating agent in the presence of a nitrogen-containing auxiliary.
摘要:
Grignard reagents which contain a protected aldehyde function are obtained in a particularly advantageous manner from a halogenated aldehyde by reaction with a secondary monoamine to give an open-chain aminal, and conversion of the latter into a Grignard reagent using metallic magnesium. The invention also relates to novel Grignard reagents of this type.