PRODUCTION OF D-(-)-TARTARIC ACID
    81.
    发明专利

    公开(公告)号:JPS63245693A

    公开(公告)日:1988-10-12

    申请号:JP7749587

    申请日:1987-04-01

    Abstract: PURPOSE:To industrially and advantageously obtain D-(-)-tartaric acid useful in the field of organic chemistry, by cultivating a specific microorganism in a culture fluid containing DL-tartaric acid. CONSTITUTION:A microorganism, such as Pseudomonas subtilis ATCC17642, belonging to the genus Pseudomonas and having the ability to assimilate L-(+)- tartaric acid without assimilating D-(-)-tartaric acid is inoculated into a culture fluid containing DL-tartaric acid in 1-300g/l concentration and cultivated at 20-35 deg.C for about 30hr by aerating and stirring at 0.5-2VVM aeration flow rate while regulating pH to 7-8. The L-(-)-tartaric acid is then asymmetrically decomposed and wholly consumed by cultivation to centrifuge the culture fluid. Microbial cells are removed to provide a supernatant liquid. CaCl2 is added to the supernatant liquid to form calcium D-(-)-tartrate. H2SO4 is subsequently added to the resultant salt to remove Ca and the obtained aqueous solution of the D-(-)-tartaric acid is then concentrated and purified.

    ALPHA-(DIPHENYLMETHYLENEAMINO)BUTYROLACTONE AND ITS PREPARATION

    公开(公告)号:JPS58150582A

    公开(公告)日:1983-09-07

    申请号:JP3228882

    申请日:1982-03-03

    Abstract: NEW MATERIAL:A compound shown by the formulaI. USE:An intermediate for synthesizing an amino acid. PROCESS:A compound shown by the formula II (R is lower alkyl) is reacted with ethylene oxide in a molar ratio of 1:(1-1.2) in a solvent such as an alcohol in the presence of 0.001-6mol equivalent base (e.g., sodium ethylate, butyl lithium) based on 1mol compound shown by the formula II at

    ETHANOLAMINE DERIVATIVE AND ITS PREPARATION

    公开(公告)号:JPS58150553A

    公开(公告)日:1983-09-07

    申请号:JP3294182

    申请日:1982-03-02

    Abstract: NEW MATERIAL:N-(Diphenylmethylene)-2-cyanoethanolamine of formulaI. USE:Useful as a synthetic intermediate of amino acids. It can be prepared with simple operation in high yield. PROCESS:The compound of formulaIcan be prepared by reacting N -(diphenyl- methylene)glycinonitrile of formula II with formaldehyde and/or paraformaldehyde preferably by an interfacial reaction of two phases solvent system, in the presence of a base such as sodium hydroxide, sodium carbonate, etc., more preferably in the presence of a phase transfer catalyst (e.g. tetrabutylammonium hydrogen sulfate, etc.) at 0-80 deg.C, preferably 0-40 deg.C under normal pressure for 5-120min.

    PREPARATION OF 2-AMINOBUTYRIC ACID DERIVATIVE

    公开(公告)号:JPS57188549A

    公开(公告)日:1982-11-19

    申请号:JP7223381

    申请日:1981-05-15

    Abstract: PURPOSE:To prepare the titled compound with simplified synthesis steps, in high yield, by reacting N-(diphenylmethylene)glycine ester with acrylonitrile, hydrolyzing the product in the presence of an acid, and further hydrolyzing in the presence of a base. CONSTITUTION:The objective compound of formula IV is prepared by (1) reacting the N-(diphenyl-methylene)glycine ester of formulaI(R is 1-4C alkyl) with acrylonitrile in the presence of a base such as sodium hydroxide at the interface of an aqueous phase and an organic phase at 0-40 deg.C, (2) hydrolyzing the resultant 2-aminobutyric acid derivative of formula II in the presence of an acid such as sulfuric acid, acetic acid, etc., to obtain the 2-aminobutyric acid derivative of formula III, and (3) hydrolyzing the product in the presence of a base such as sodium hydroxide.

    7,9,10,12-TETRAAZATRICYCLO(4,3,3)DODECANE-8,11-DITHION AND ITS PREPARATION

    公开(公告)号:JPS57154185A

    公开(公告)日:1982-09-22

    申请号:JP3993381

    申请日:1981-03-19

    Abstract: NEW MATERIAL:7,9,10,12-Tetraazatricyclo[4,3,3]dodecane-8,11-dithion shown by the formulaI(n is 0 or 1) or its N-methylpyrrolidone complex. USE:An intermediate for drug, industrial rubber chemical, or its intermediate. A polymer modifier and rust preventive. PROCESS:An alpha-aminocyclohexanone oxime is reacted with a metal thiocyanate (e.g., sodium thiocyanate) or ammonium thiocyanate in the presence of acetic acid, to give 7,9,10,12-tetraazatricyclo[4,3,3] dodecane-8,11-dithion shown by the formula II wherein n is 0 in the formulaI, this compound is further reacted with N-methylpyrrolidone to give a dithion complex shown by the formula III wherein n is 1 in the formulaI.

    N-(DIPHENYLMETHYLENE) TRYPTOPHAN ESTER

    公开(公告)号:JPS57154165A

    公开(公告)日:1982-09-22

    申请号:JP3993281

    申请日:1981-03-19

    Abstract: NEW MATERIAL:The N-(diphenylmethylene)tryptophan ester of formulaI(R is 1-4C alkyl). EXAMPLE:N-(Diphenylmethylene)tryptophan ethyl ester. USE:Raw material for the perparation of tryptophan. Tryptophan can be produced from the ester with easy synthetic process, in high yield, under mild reaction conditions. PROCESS:The compound of formula can be prepared, e.g. by reacting the N- (diphenyl-methylene)glycine ester of formula II with the (3-indolylmethyl)trimethylammonium methylsulfate of formula III. The compound can be converted to tryptophan of formula IV either by hydrolyzing with an acid and successively with a base, or by hydrolyzing with a base and successively with an acid.

    1*6*111TRIS DIMETHYLAMINO UNDECANE
    87.
    发明专利

    公开(公告)号:JPS5646848A

    公开(公告)日:1981-04-28

    申请号:JP12257579

    申请日:1979-09-26

    Abstract: NEW MATERIAL:1,6,11-Tris(dimethylamino)undecane expressed by formula I. USE:Industrially useful as a blowing catalyst for urethane, a curing accelerator for an epoxy resin, a textile modifier or a raw material for fine chemicals. PROCESS:1,6,11-Triaminoundecane (A) expressed by formula II is, directly or in an aqueous solution, fed to a mixture solution of formaldehyde in an amount of 6mol based on 1mol of (A) with formic acid in an amount of 9mol based on 1mol of (A), according to the formula, preferably at 70-105 deg.C, to give the titled compound expressed by formula I. A reaction solvent is not particularly required but the reaction proceeds very smoothly in the presence of water. The titled compound is a liquid at ordinary temperature, easily handleable due to its low vapor pressure, and has little bad effects on man.

    PURIFICATION OF TERTIARY AMINE
    88.
    发明专利

    公开(公告)号:JPS55143938A

    公开(公告)日:1980-11-10

    申请号:JP5090479

    申请日:1979-04-26

    Abstract: PURPOSE:To purify a tertiary amine and, in some cases, to improve its yield, by reacting formaldehyde (derivatives) remaining in the tertiary amine with ammonia under basic conditions. CONSTITUTION:A tertiary amine is, obtained by the reductive methylation of a primary or secondary amine with formaldehyde and formic acid or formaldehyde and hydrogen. On this occasion, formaldehyde and/or formaldehyde derivatives remaining in the tertiary amine is reacted with ammonia under basic conditions, and the separated tertiary amine is purified. The amount of ammonia used is preferably such an amount that the amount of the free ammonia existing in the system is at least equivalent to remove the formaldehydes and, at the same time, pH of the system becomes at least 8. When the desired tertiary amine has functional groups, the yield of the desired substance can be improved by this process. EFFECT:Neutralization, separation and removal of formaldehyde can be corried out at the same time.

    PREPARATION OF BASIC POLYAMIDE
    89.
    发明专利

    公开(公告)号:JPS5592736A

    公开(公告)日:1980-07-14

    申请号:JP85879

    申请日:1979-01-05

    Abstract: PURPOSE:To obtain a basic polyamide soluble in organic solvents, e.g. methanol, and water, by polymerizing an alpha-(N,N-dialkylamino)-epsilon-caprolactam in the presence of a basic catalyst. CONSTITUTION:(A) An alpha-(N,N-dialkylamino)-epsilon-caprolactam or in combination with (B) a cyclic amid, e.g. epsilon-caprolactam, of the formula (n is 3-11) is polymerized in the presence of (C) a basic catalyst, preferably metallic lithium, sodium, or potassium, triethylaluminum, or diethylzinc, if necessary (D) a co-catalyst, e.g. N-acetyl-epsilon-caprolactam. The molar ratio of (A) to (A+B) is >=0.1, and that of (C+D) to (A+B) is 1:20-500. USE:Sizes, paper strength improvers, adehesives, and coating materials.

    ALPHAASUBSTITUTED AMINOOEPSILONNCAPROLACTAM

    公开(公告)号:JPS5528938A

    公开(公告)日:1980-02-29

    申请号:JP10196178

    申请日:1978-08-22

    Abstract: NEW MATERIAL:An alpha-substituted amino-epsilon-caprolactam of the formula (R1 is CH2CH2OH; R2 is H or CH2CH2OH). EXAMPLE:alpha-(2-Hydroxyethylamino)-epsilon-caprolactam. USE:Pesticides, raw materials for high polymers, epoxy curing agents, and intermediates for them or other compounds. PROCESS:alpha-Amino-epsilon-caprolactam, obtained by amination of alpha-chloro-epsilon-caprolactam, is reacted with ethylene chloro hydrin or ethylene oxide in a solvent, e.g. water, analcohol, or chloroform, at room temperature- 160 deg.C to give the compound of the formula.

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