摘要:
Phthalides in as-obtained phthalide synthesis reaction mixtures are recovered in pure form by (a) distilling compounds having a boiling point below the boiling point of the phthalide from the reaction mixture, provided such compounds are present in the reaction mixture, to obtain a crude phthalide as bottom product, (b) crystallizing the phthalide from a melt of the crude phthalide.
摘要:
A process for preparing phthalides by I. reducing phthalic acid or phthalic acid derivatives, where the carboxyl groups may be replaced by units which can be derived from the carboxyl groups by a condensation reaction and where one or more of the hydrogens of the o-phenylene unit may be substituted by inert radicals, at a cathode in a undivided electrolytic cell and dissolved in an electrolyte, II. discharging the electrolyte from the electrolytic cell when the reaction has proceeded to the stage where the molar ratio (M), formed by the proportion of phthalide and the sum of the proportions of phthalide and phthalic acid of phthalic acid derivatives in the electrolyte, is from 0.8:1 to 0.995:1, and III. crystallizing the phthalides from the electrolyte and removing them from the mother liquor, if appropriate after distillative work-up of the electrolyte is described.
摘要:
A process for the selective hydrolysis of acetals in the presence of phthalides comprises reacting a mixture (M) comprising a) a phthalide of the formula (I) where: R1,R2,R3 and R4: are independently hydrogen, C1-C4-alkyl or halogen, and b) an acetal or ketal of the formula (II) where: R5 and R6: are independently C1-C6-alkyl, C6-C10-aryl or together ethylene, and R7 and R8: are independently C1-C6-alkyl, or one radical is a hydrogen and the other is a phenyl radical where from 1 to 3 hydrogen atoms of the phenyl radical may be replaced by C1-C6-alkyl radicals or C1-C4-alkoxy radicals, or R7 and R8 are together C3-C6-alkanediyl, and a hydrogen atom may be replaced by a hydroxyl group, at from 10 to 200° C. in the presence of from 1 to 10 mol of water, based on the amount of acetal or ketal of the formula (II), to hydrolyze the acetal or ketal of the formula (II) to the corresponding aldehyde or ketone.
摘要:
A method for producing alcoxylated carbonyl compounds of general formula (I) (compounds I): R1aR2C(OR3)b wherein R1, R2 represent hydrogen or C1-C6-alkyl, R3 independently means C1-C6-alkyl, a is 0 or 1, b 2 or 3 with the proviso that the sum of a and b is 3, by means of anodic oxidation of germinal dialcoxy compounds of general formula (II) (compounds II) wherein R4, R5, R6, R7 represent hydrogen or C1-C6-alkyl, R5, R6 represent C1-C6-alkyl or C1-C6-alcoxy, in the presence of a C1-C6-alkyl alcohol (compounds III). A usual compound (compound IV) is used as a cathodic depolarizer suitable for electrochemical oxidation. The anodic oxidation and cathodic reduction is carried out in an undivided electrolyte cell in the presence of C1-C6-alkyl alcohols.
摘要:
A process is described for preparing diacetals of glyoxal by reacting from 40 to 75% by weight aqueous glyoxal with monohydric alcohols in the presence of an acid catalyst, which comprises leaving a liquid mixture which, at the beginning of the reaction, comprises alcohol and glyoxal in a molar ratio of at least 15:1 and also water in a concentration of not more than 8% by weight in contact with the acid catalyst until concentration in the reaction mixture of the diacetal formed reaches at least 70% of the equilibrium concentration without more than 5% by weight of the alcohol used having already been distilled off.
摘要:
The present invention relates to a process for preparing a porous metal organic framework comprising at least two organic compounds coordinated to at least one metal ion, which comprises the steps (a) oxidation of at least one anode comprising the metal corresponding to at least one metal ion in a reaction medium in the presence of at least one first organic compound which is an optionally substituted monocyclic, bicyclic or polycyclic saturated or unsaturated hydrocarbon in which at least two ring carbons have been replaced by heteroatoms selected from the group consisting of N, O and S to form a reaction intermediate comprising the at least one metal ion and the first organic compound; and (b) reaction of the reaction intermediate at a prescribed temperature with at least one second organic compound which coordinates to the at least one metal ion, with the second organic compound being derived from a dicarboxylic, tricarboxylic or tetracarboxylic acid.
摘要:
In a process for producing an alkali metal from alkali metal amalgam by electrolysis using an alkali metal amalgam as anode, a solid electrolyte which conducts alkali metal ions and a liquid alkali metal as cathode, the alkali metal amalgam as anode is kept in motion.
摘要:
A process for producing metallic lithium starting from an aqueous solution of at least one lithium salt comprises the following steps: (I) Production of a lithium amalgam from an aqueous solution of at least one lithium salt; and (II) Electrolysis using an anode comprising the lithium amalgam, a solid electrolyte which conducts lithium ions, and liquid lithium as cathode, wherein the lithium amalgam as anode is kept in motion.
摘要:
The present invention relates to a process for preparing a porous metal organic framework comprising at least two organic compounds coordinated to at least one metal ion, which comprises the steps (a) oxidation of at least one anode comprising the metal corresponding to at least one metal ion in a reaction medium in the presence of at least one first organic compound which is an optionally substituted monocyclic, bicyclic or polycyclic saturated or unsaturated hydrocarbon in which at least two ring carbons have been replaced by heteroatoms selected from the group consisting of N, O and S to form a reaction intermediate comprising the at least one metal ion and the first organic compound; and (b) reaction of the reaction intermediate at a prescribed temperature with at least one second organic compound which coordinates to the at least one metal ion, with the second organic compound being derived from a dicarboxylic, tricarboxylic or tetracarboxylic acid.
摘要:
A process for preparing butanetetracarboxylic acid derivatives as product of value I by coupled electrosynthesis which comprises cathodically reducing a compound selected from the group consisting of maleic esters, maleic ester derivatives, fumaric esters and fumaric ester derivatives where at least one hydrogen atom in positions 2 and 3 may be replaced by inert groups and obtaining a product of value II at the node.