Abstract:
The invention relates to a method for the purification of triazolylmethylepoxide isomers of formula (I), where A and B independently = C1-C4 alkyl, phenyl-(C1-C2 alkyl), C3-C6 cycloalkyl, C3.C6 cycloalkenyl, tetrahydropyranyl, tetrahydrofuranyl, dioxanyl or phenyl, whereby the phenyl residue can carry one to three substituent from the group: halogen, nitro, C1-C4 alkyl, C1-C4 alkyloxy, phenoxy, amino, C1-C2 haloalkyl or phenylsulphonyl obtained by reaction of an epoxide of formula (II), where A and B have the above given meanings and L is a nucleophilic leaving group, with a) a 1, 2, 4-triazole (IIIa) and a molar equivalent of an inorganic base or b) 1,2,4-triazolide of formula (IIIb), (IIIa): Me = H, IIIb: alkali metal, in which Me = an alkali metal atom or a quaternary ammonium ion, in an aprotic, dipolar solvent, characterised in that, at the end of the reaction, the reaction solution is treated with a water-miscible co-solvent and the triazolylmethylepoxide isomers are fractionally precipitated with water.
Abstract:
The invention relates to a method for producing triazolyl methyl oxiranes of formula I wherein A and B are the same or different and independently represent C1-C4-alkyl, phenyl-C1-C2-alkyl, C3-C6-cycloalkyl, C3-C6-cycloalkenyl, tetrahydropyranyl, tetrahydrofuranyl, dioxanyl or phenyl, the phenyl radical being able to carry between one and three substituents selected from the group containing halogen, nitro, C1-C4-alkyl, C1-C4-alkoxy, phenoxy, amino, C1-C2-halogenalkyl or phenylsulfonyl. Said compounds are produced by converting an oxirane of formula II wherein A and B have the aforementioned designation, and L represents a leaving group which can be substituted in a nucleophilic manner, with a) 1,2,4-triazole (IIIa) and a molar equivalent of an inorganic base, or b) a 1,2,4-triazolide of formula IIIb wherein Me represents an alkali metal atom or a quaternary ammonium ion, in a dipolar aprotic solvent having an OH-acid compound content of less than 0.5 % and/or having an NH-acid compound content of less than 2.5 %.
Abstract:
The invention relates to a method for producing isocyanates by reacting amines with phosgene inside a reactor followed by separating the isocyanate out from the reaction mixture exiting the reactor and purifying this isocyanate. The invention is characterized in that the isocyanate is separated out and purified in a column with a top pressure of 1 to 950 mbar, preferably 5 to 50 mbar, particularly preferred 10 to 20 mbar, with a bottom temperature of 90 to 250 °C, preferably 120 to 170 °C, particularly preferred 130 to 150 °C, and that the pure isocyanate flow is withdrawn in liquid or gaseous form, preferably in a side-stream of the column.
Abstract:
The invention relates to a method for producing amines by hydrogenating nitro compounds and is characterized in that the hydrogenation is carried out in a vertical reactor whose diameter is larger than its length. The reactor comprises a jet nozzle which is arranged in the upper area of the reactor and which is directed downwards. The educts and the reaction mixture are delivered via said jet nozzle. The reactor also comprises an outlet situated in any position of the reactor via which the reaction mixture in an outer circuit is delivered once again to the jet nozzle by means of a conveying organ, and the reactor has a flow reverse situated in the lower area of the reactor.
Abstract:
The invention relates to a method for treating distillation residues from the synthesis of toluene diisocyanate by reacting the distillation residues with water. The invention is characterized in that the TDI distillation residues are reacted with water in a continuos or semi-continuos method in a back-mixed reactor in the presence of hydrolyzates.
Abstract:
The invention relates to a method for the production of 1,2,4-triazol-1-yl-methyl-oxiranes of formula (I) wherein A and B are the same or different and independently represent C1-C4-alkyl, phenyl-C1-C2-alkyl,. C3 --C6-cycloalkyl, C3-C6-cycloalkenyl, tetrahydropyranyl, tetrahydrofuranyl, dioxanyl or phenyl. The phenyl radical can contain 1 3 substituents selected form the group: halogen, nitro, C1-C4-alkyl, C1-C4-alkyloxy, phenoxy, amino, C1-C2-halogenalkyl or phenylsulfonyl, characterised in that a) an oxirane of formula (II) wherein A and B have the above mentioned meaning and L represents a nucleophilically substitutable leaving group which is reacted with 4-amino-1,2,4-triazol of formula (III), IV to form 4-amino-1,2,4-triazolium salts of formula (IV). The invention also relates to a method for the production of l,2,4-triazolylmethyl-oxiranes.
Abstract:
The invention relates to a method for producing triazolyl methyl oxiranes of formula I wherein A and B are the same or different and independently represent C1-C4-alkyl, phenyl-C1-C2-alkyl, C3-C6-cycloalkyl, C3-C6-cycloalkenyl, tetrahydropyranyl, tetrahydrofuranyl, dioxanyl or phenyl, the phenyl radical being able to carry between one and three substituents selected from the group containing halogen, nitro, C1-C4-alkyl, C1-C4-alkoxy, phenoxy, amino, C1-C2-halogenalkyl or phenylsulfonyl. Said compounds are produced by converting an oxirane of formula II wherein A and B have the aforementioned designation, and L represents a leaving group which can be substituted in a nucleophilic manner, with a) 1,2,4-triazole (IIIa) and a molar equivalent of an inorganic base, or b) a 1,2,4-triazolide of formula IIIb wherein Me represents an alkali metal atom or a quaternary ammonium ion, in a dipolar aprotic solvent having an OH-acid compound content of less than 0.5 % and/or having an NH-acid compound content of less than 2.5 %.
Abstract:
The invention relates to a method for producing amines by hydrogenating nitro compounds and is characterized in that the hydrogenation is carried out in a vertical reactor whose diameter is larger than its length. The reactor comprises a jet nozzle which is arranged in the upper area of the reactor and which is directed downwards. The educts and the reaction mixture are delivered via said jet nozzle. The reactor also comprises an outlet situated in any position of the reactor via which the reaction mixture in an outer circuit is delivered once again to the jet nozzle by means of a conveying organ, and the reactor has a flow reverse situated in the lower area of the reactor.
Abstract:
The invention relates to a method for treating distillation residues from the synthesis of toluene diisocyanate by reacting the distillation residues with water. The invention is characterized in that the TDI distillation residues are reacted with water in a continuos or semi-continuos method in a back-mixed reactor in the presence of hydrolyzates.
Abstract:
The invention relates to a method for the production of 1,2,4-triazol-1-yl-methyl-oxiranes of formula (I) wherein A and B are the same or different and independently represent C1-C4-alkyl, phenyl-C1-C2-alkyl,. C3 --C6-cycloalkyl, C3-C6-cycloalkenyl, tetrahydropyranyl, tetrahydrofuranyl, dioxanyl or phenyl. The phenyl radical can contain 1 3 substituents selected form the group: halogen, nitro, C1-C4-alkyl, C1-C4-alkyloxy, phenoxy, amino, C1-C2-halogenalkyl or phenylsulfonyl, characterised in that a) an oxirane of formula (II) wherein A and B have the above mentioned meaning and L represents a nucleophilically substitutable leaving group which is reacted with 4-amino-1,2,4-triazol of formula (III), IV to form 4-amino-1,2,4-triazolium salts of formula (IV). The invention also relates to a method for the production of l,2,4-triazolylmethyl-oxiranes.