摘要:
Method of producing compounds of the general formula XPR2(OR1) Ia where X is chlorine, bromine or iodine and R1 is an organic radical, by reacting compounds of the general formula X2PR2 II, in which X has the meaning given above and R2 is an organic radical, with compounds of the general formula R1OH III, in which R1 has the meaning given above, to give a mixture IV, in that a) the postreaction is carried out at a temperature of from 50 to 240° C. and a pressure of from 0.001 to 0.9 bar, b) from the mixture IV the compounds Ia are separated off from the compounds PR2(OR1)2 Ib and, if appropriate, the compounds II and c) compounds Ib and, if appropriate, unreacted compounds II are returned to the synthesis stage.
摘要:
A process for extractively removing nickel(0) complexes having phosphorus ligands from a reaction effluent of a hydrocyanation of unsaturated mononitriles to dinitriles by extraction by means of a hydrocarbon, a phase separation of the hydrocarbon and of the nitrile-containing solution into two phases being effected, by feeding at least one polar additive to the hydrocyanation effluent (feedstream) and/or to the extraction stage.
摘要:
A method for producing 3-pentenenitrile by means of the hydrocyanation of 1,3-butadiene, which comprises the following process steps: (b′) distillation of 1,3-butadiene comprising water, 1- and 2-butenes and a stabilizer in a distillation apparatus K4 to obtain a stream 15 as the bottom product, which comprises dried 1,3-butadiene, 1- and 2-butenes and the stabilizer, and a stream 16 as the top product, which comprises an azeotropic 1,3-butadiene/water mixture, condensation of the stream 16 in a condenser W, transfer of the resulting condensate (stream 17) into a phase separation apparatus, recycling of the upper liquid phase (stream 18) consisting of 1,3-butadiene as reflux to the column K4, and discharge of the lower liquid aqueous phase (stream 19), (a) reaction of stream 15 in a reactor R1 with hydrogen cyanide over at least one catalyst (stream 6d) to obtain a stream 1 which comprises 3-pentenenitrile, 2-methyl-3-butenenitrile, the at least one catalyst, unconverted 1,3-butadiene, and 1- and 2-butenes, with or without residues of unconverted hydrogen cyanide, (b) distillation of stream 1 in a distillation apparatus K1 to obtain a stream 2 as the top product, which comprises the predominant portion of the 1,3-butadiene from stream 1, and to obtain a stream 3 as the bottom product, which comprises 3-pentenenitrile, the at least one catalyst, 2-methyl-3-butenenitrile, 1- and 2-butenes and the remaining proportion of the 1,3-butadiene from stream 1 which has not been removed in stream 2, (c) distillation of stream 3 in a distillation apparatus K2 to obtain a stream 5 at a side draw of the column, which 3-pentenenitrile and 2-methyl-3-butenenitrile, a stream 6 as the bottom product, which comprises the at least one catalyst, and a stream 4 as the top product, (d) compression of stream 4 in the compressor V1, discharge of a gaseous substream 4b which comprises 1- and 2-butenes, transfer of the compressed stream 4a into the condenser W1, combined cond. With stream 2 from b) in combined condensation of this stream 2 from b) and transfer of the condensate as stream 9, partly as reflux to the column K1 (stream 9b), partly as return stream into the reactor R1 (stream 9a), and (e) distillative separation of stream 5 to obtain 3-pentenenitrile and 2-methyl-3-butenenitrile.
摘要:
A process for preparing nickel(0)-phosphorus ligand complexes comprising at least one nickel(0) central atom and at least one phosphorus ligand by reacting a nickel(II) compound with a reducing agent in the presence of the ligand to give a reaction mixture, wherein a) the molar reducing agent:nickel(II) compound ratio in the reaction is from 1:1 to 1000:1, calculated as the molar ratio of the redox equivalents, b) the molar phosphorus ligand:nickel(II) compound ratio in the reaction is not more than 30:1, calculated as the molar P atoms:Ni atoms ratio, c) the nickel(0) content in the resulting reaction mixture is not more than 1.3% by weight and d) the resulting reaction mixture is extracted by adding at least one dinitrile and at least one hydrocarbon to form at least two immiscible phases.
摘要:
A process for preparing urethanes by reacting aromatic diamines with a dialkyl carbonate, wherein the alkyl radical of the organic dialkyl carbonate comprises 2-18 carbon atoms and one or more heteroatoms and the reaction is performed in the presence of a catalyst.
摘要:
The invention provides metal carbamates of the general formula (I) where R1 and R2 are the same or different and are each an alkyl group having 1-18 carbon atoms and M is an alkali metal atom.
摘要:
A process for the production of compounds Ar—R1 by means of a cross-coupling reaction of an organometallic reagent R1-M with an aromatic or heteroaromatic substrate Ar—X catalyzed by one or several iron salts or iron complexes as catalysts or pre-catalysts, present homogeneously or heterogeneously in the reaction mixture. This new invention exhibits substantial advantages over established cross coupling methodology using palladium- or nickel complexes as the catalysts. Most notable aspects are the fact that (i) expensive and/or toxic nobel metal catalysts are replaced by cheap, stable, commercially available and toxicologically benign iron salts or iron complexes as the catalysts or pre-catalysts, (ii) commercially attractive aryl chlorides as well as various aryl sulfonates can be used as starting materials, (iii) the reaction can be performed under “ligand-free” conditons, and (iv) the reaction times are usually very short.
摘要:
A process for preparing urethanes by reacting aromatic diamines with a dialkyl carbonate, wherein the alkyl radical of the organic dialkyl carbonate comprises 2-18 carbon atoms and one or more heteroatoms and the reaction is performed in the presence of a catalyst.
摘要:
The object of the invention is to provide a process for preparing urethanes by reacting aromatic amines with a dialkyl carbonate, wherein the alkyl radical of the organic dialkyl carbonate comprises from 2 to 18 carbon atoms, and the reaction is carried out in the presence of a base.