Abstract:
A method for making an optically active 3- aminopyrrolidine-2,5-dione derivative represented by the formula (3) includes cyclizing an optically active asparagine ester derivative represented by the formula (1) or (2), or an acid salt thereof. A method for making an optically active 3-aminopyrrolidine derivative represented by the formula (9) includes reducing the optically active 3- aminopyrrolidine-2,5-dione derivative represented by the formula (3). A method for making an optically active 3- aminopyrrolidine derivative includes hydrogenolyzing the optically active 3-aminopyrrolidine derivative represented by the formula (9).
Abstract:
A method for making an optically active 3- aminopyrrolidine-2,5-dione derivative represented by the formula (3) includes cyclizing an optically active asparagine ester derivative represented by the formula (1) or (2), or an acid salt thereof. A method for making an optically active 3-aminopyrrolidine derivative represented by the formula (9) includes reducing the optically active 3- aminopyrrolidine-2,5-dione derivative represented by the formula (3). A method for making an optically active 3- aminopyrrolidine derivative includes hydrogenolyzing the optically active 3-aminopyrrolidine derivative represented by the formula (9).
Abstract:
PROBLEM TO BE SOLVED: To readily purify a ketonic acid ester into a high purity at a low cost by heating a mixture containing the ketonic acid ester and a hydroxy acid ester in the coexistence of an acid. SOLUTION: A mixture containing (A) a ketonic acid ester (preferably an α-ketonic acid ester, e.g. a pyruvic acid ester) and (B) a hydroxy acid ester (preferably an α-hydroxy acid ester, e.g. a lactic acid ester) is heated in the coexistence of (C) an acid (preferably sulfuric acid, an aromatic sulfonic acid or an aliphatic sulfonic acid) (preferably at 30-90 deg.C) to thereby purify the ketonic acid ester of the component (A). Ester residues of the components (A) and (B) are the same and preferably 1-6C alkyls. Furthermore, the component (C) preferably coexists in an amount of 1-500mol% based on the component (B). The weight ratio of the components (A) to (B) is preferably (1000/1) to (5/1).
Abstract:
PURPOSE:To easily and directly obtain the subject compound with single-stage operation in high yield on an industrial scale at a low cost by using nitrosyl chloride soluble in organic solvent as a nitrosation agent and reacting diphenylamines with the nitrosation agent and hydrogen chloride in a specific solvent to effect the nitrosation of the diphenylamines. CONSTITUTION:The objective compound of formula II useful as an intermediate for antioxidant for rubber, azo dye, etc., is produced by the nitrosation reaction of diphenylamines of formula I (R and R are H, CH3, C2H5, cyclohexyl, OCH3, OC2H5, C1 or Br) with nitrosyl chloride and hydrogen chloride in a solvent containing 1-10C alkyl alcohol (e.g., isobutanol) or a cycloalcohol usually at 5-60 deg.C under atmospheric pressure. The nitrosyl chloride used as the nitrosation agent is free from explosion or decomposition property and has little problems in handling. The amount of hydrogen chloride can be decreased because the hydrogen chloride produced from nitrosyl chloride can be used as it is in the reaction.
Abstract:
The present invention provides a process to produce fine particles of polyamide-imide resin that can be carried out industrially by simple operations with a high reproducibility. It also provides very fine PAI resin particles with a uniform particle size. The invention provides a production process for fine PAI resin particles comprising a dissolution steps and a precipitation step as described below: [Dissolution step] A step selected from the undermentioned steps (a1) and (b1) (a1) PAI resin is dissolved in an organic solvent to prepare a PAI resin solution A1 having a PAI resin content of less than 5 mass%, (b1) PAI resin is dissolved in an organic solvent to prepare a PAI resin solution B1 having a PAI resin content of less than 10 mass%. [Precipitation step] (a2) The PAI resin solution A1 is added to a solvent that is virtually free from surface active agents and able to precipitate fine PAI resin particles, in order to cause the precipitation of fine PAI resin particles, (b2) The PAI resin solution B1 is subjected to flash crystallization to cause the precipitation of fine PAI resin particles.
Abstract:
PROBLEM TO BE SOLVED: To obtain an aspartic acid dibenzyl ester-sulfonate having high purity with simple procedure by purifying a crude aspartic acid dibenzyl ester-sulfonate in an organic solvent containing a specific amount of water. SOLUTION: The objective compound is produced by purifying (A) a crude aspartic acid dibenzyl ester-sulfonate of formula (R1 and R2 are each H, a 1-4C lower alkyl, a 1-4C lower alkoxy or a halogen; R3 is H or a 1-3C lower alkyl and the substitution position may be ortho, meta or para; (n) is 0-2) is (B) an organic solvent containing >=2 times mol of water based on the component A. The purification procedure of the component A depends upon the content of water-soluble impurities. For example, when the component A contains only a small amount of water-soluble impurities, the procedure is carried out by suspending the component in an organic solvent, adding >=2 times mol of water based on the component A while stirring the suspension at a prescribed temperature, cooling the product, separating the precipitated crystal by filtration and drying the crystal.
Abstract:
PROBLEM TO BE SOLVED: To provide a method for producing an α-ketocarboxylic acid ester by oxidizing a specific α-hydroxycarboxylic acid ester with hypochlorous acid in the presence of a specified hindered secondary amine under an acidic condition, capable of producing the α-ketocarboxylic acid ester from the general chemical agents in a high yield under as mild conditions as possible. SOLUTION: The method for producing an α-ketocarboxylic acid ester comprises oxidizing an α-ketocarboxylic acid ester of formula I [R is an alkyl, a cycloalkyl, a (substituted) aryl or an aralkyl; R is a 1-4C alkyl] (for example, methyl lactate or ethyl lactate) with hypochlorous acid in the presence of a hindered secondary amine of formula II (R is H, a
Abstract:
PURPOSE:To isolate a natural type abscisic acid being an important compound as a natural plant hormone and capable of expecting wide uses such as plant growth regrator, etc., in high purity and yield from a solution containing the natural type abscisic acid by carrying out the isolation operation of the natural type abscisic acid in a state in which light having a specific wavelength is blocked. CONSTITUTION:A natural type abscisic acid is isolated in high yield from a solution containing the natural type abscisic acid by carrying out isolation operation of the natural type abscisic acid in a state in which light having 200-600nm wavelength is blocked. This isolation is preferably carried out under conditions at pH1-11 and temperature of 0-60 deg.C. An >=80% of total isolation operation based on time is preferably carried out in a state in which light having 200-600nm wavelength is blocked. Furthermore, the natural type abscisic acid(ABA) is (+)-cis-trans type expressed by the formula. The isomerization and decomposition of ABA are suppressed and recovery of ABA is enhanced and ABA can efficiently be isolated by this method. Further, since the isolated ABA is not isolated or decomposed even in successive operation, high-purity ABA is readily obtained.
Abstract:
PURPOSE:To efficiently and selectively isolate abscisic acid from a dilute solution containing the abscisic acid in high yield without concentrating an organic layer extracted with an organic solvent by reducing the amount of the organic solvent used. CONSTITUTION:The method for isolating abscisic acid is characterized by comprising an extraction step for bringing an aqueous solution containing the abscisic acid into contact with an organic solvent immiscible with water and making the abscisic acid pass into the organic solvent, a back extraction step for bringing the organic layer, separated from the extraction step and containing the abscisic acid into contact with an aqueous solution of an alkali and making the abscisic acid pass into the aqueous solution of the alkali, a recycling step for recycling the organic layer subjected to the back extraction of the abscisic acid in the back extraction step to the extraction step and a step for isolating the abscisic acid from the aqueous solution of the alkali, separated in the back extraction step and containing the abscisic acid. The isolated abscisic acid is capable of reducing the subsequent purification load and providing an industrially inexpensive high-purity abscisic acid (ABA).