公开(公告)号：JPS6344592A

公开(公告)日：1988-02-25

申请号：JP18775786

申请日：1986-08-12

Applicant: TOSOH CORP

Inventor： WAKAMATSU HIDETOSHI ,  IRINO SHIGEAKI ,  HARADA TSUNEO ,  TOKUDA AKIRA ,  KOYAMA KIYOTAKA

IPC: A23L27/30 ,  C07K1/14 ,  C07K5/072 ,  C07K5/075

Abstract: PURPOSE:To suppress formation of type II crystals by drying and obtain the titled compound useful as sweeteners, etc., by granulating wet crystals of alpha-L- aspartyl-L-phenylalanine methyl ester under specific condition and drying the resultant granulated crystals. CONSTITUTION:Wet crystals of alpha-L-aspartyl-L-phenyalanine methyl ester are initially granulated to give >=4m /g specific surface area after drying and the resultant granulated crystals are dried, preferably at =4m /g.

公开(公告)号：JPH01149740A

公开(公告)日：1989-06-12

申请号：JP30756987

申请日：1987-12-07

Applicant: TOSOH CORP

Inventor： OKIZAKI AKIO ,  KUBO MASAJI ,  FUJII SATOSHI ,  KOYAMA KIYOTAKA

IPC: C07B61/00 ,  B01J21/06 ,  B01J23/06 ,  B01J23/14 ,  B01J23/18 ,  B01J27/10 ,  B01J27/135 ,  C07C17/00 ,  C07C17/12 ,  C07C25/18 ,  C07C67/00

Abstract: PURPOSE:To obtain the title compound in high yield, high selectivity, in a short time and readily in brominating biphenyl with bromine, by using a specific amount of bromine in a halogenated hydrocarbon solvent in the presence of an antimony, titanium, tin or zinc catalyst. CONSTITUTION:Biphenyl is reacted with 2-3mol based on 1mol biphenyl of bromine in a halogenated hydrocarbon solvent in the presence of a catalyst of an element simple substance of antimony, titanium, tin or zinc or a compound thereof such as a halide, oxide, hydroxide, inorganic salt and/or organic salt, preferably halide to give 4,4'-dibromobiphenyl useful as a raw material for biphenyl-4,4'-diol (monomer for engineering plastics, antioxidant and intermediate for dye) in high selectivity, high yield and in easy reaction control.

公开(公告)号：JPS63166434A

公开(公告)日：1988-07-09

申请号：JP31017186

申请日：1986-12-29

Applicant: TOSOH CORP

Inventor： NAKANO MASAO ,  SEKIZAWA KAZUHIKO ,  HIRONAKA TOSHIO ,  KOYAMA KIYOTAKA ,  ASANO SEIICHI

IPC: B01J29/06 ,  B01J29/08 ,  B01J29/50 ,  B01J29/60 ,  C07B39/00 ,  C07B61/00 ,  C07C17/00 ,  C07C17/12 ,  C07C25/02 ,  C07C67/00 ,  C10G35/10

Abstract: PURPOSE:To enhance activity and to facilitate separation and recovery of a catalyst by forming the zeolite catalyst in such spherical bodies that these have specified particle diameter and pores of a specified range and the volume of the pores is regulated in a specified range and also the diameter of median pore is regulated in a specified range. CONSTITUTION:A zeolite catalytic molded form for liquid phase organic reaction is obtained by a spray drying granulation method wherein a slurry contg. zeolite is sprayed into hot air, it is a spherical body practically having a particle diameter in a range of 70-500mum, and the volume of pores of (0.4-1.0)cc/g in the pores of 100-75,000Angstrom to form an integral body, having, 1,000-5,500Angstrom diameter of median pore based on the volume of the narrow pores. This catalytic molded form is used as the catalyst for liquid phase organic reaction after calcining at a range of temp. within about 250-900 deg.C, and therefore the mechanical strength of the molded form is well held.

公开(公告)号：JPS6354346A

公开(公告)日：1988-03-08

申请号：JP19809686

申请日：1986-08-26

Applicant: TOSOH CORP

Inventor： HARADA TSUNEO ,  KOYAMA KIYOTAKA

IPC: C07B31/00 ,  C07B55/00 ,  C07C67/00 ,  C07C227/00 ,  C07C227/14 ,  C07C227/36 ,  C07C229/36

Abstract: PURPOSE:To complete racemization reaction within a short time under high temperature and pressure condition to cause decomposition of amino acid and to obtain racemized product at low apparatus and production costs while suppressing the formation of impurities, by heating an optically active amino acid in an aqueous solution in alkaline region in the presence of an alkali metal salt. CONSTITUTION:An optically active amino acid such as L-phenylalanine is dissolved in water and obtained aqueous solution is heated at >=100 deg.C in an alkaline region (preferably >=10pH) in the presence of an alkali metal salt (especially salt of Li, Na or K at a concentration of >=0.2M) to effect the racemization of the amino acid. The racemization proceeds at a high reaction rate without causing decomposition and polymerization of the amino acid.

公开(公告)号：JPS6345298A

公开(公告)日：1988-02-26

申请号：JP18866386

申请日：1986-08-13

Applicant: TOSOH CORP

Inventor： WAKAMATSU HIDETOSHI ,  IRINO SHIGEAKI ,  HARADA TSUNEO ,  TOKUDA AKIRA ,  KOYAMA KIYOTAKA

IPC: A23L27/30 ,  C07K1/14 ,  C07K5/06 ,  C07K5/075

Abstract: PURPOSE:To obtain type-II crystal of alpha-L-aspartyl-L-phenylalanine methyl ester having excellent storage stability without using high-temperature drying, by contacting alpha-L-aspartyl-L-phenylalanine methyl ester containing type-I crystal with a polar organic solvent. CONSTITUTION:alpha-L-aspartyl-L-phenylalanine methyl ester containing type-I crystal (having high hygroscopicity and liable to cause discoloration and decomposition during storage) can be easily converted to stable type-II crystal, by contacting the compound with a polar organic solvent (preferably 1-4C alcohol).

公开(公告)号：JPS6345296A

公开(公告)日：1988-02-26

申请号：JP18866186

申请日：1986-08-13

Applicant: TOSOH CORP

Inventor： WAKAMATSU HIDETOSHI ,  IRINO SHIGEAKI ,  HARADA TSUNEO ,  TOKUDA AKIRA ,  KOYAMA KIYOTAKA

IPC: A23L27/30 ,  C07K1/14 ,  C07K5/072 ,  C07K5/075

Abstract: PURPOSE:To obtain an aspartame having excellent storage stability without using high-temperature drying process, by heat-treating an alpha-L-aspartyl-L- phenylalanine methyl ester crystal having a specific water content under a specific condition. CONSTITUTION:Stable alpha-L-aspartyl-L-phenylalanine methyl ester can be produced by heat-treating an alpha-L-aspartyl-L-phenylalanine methyl ester crystal containing 5-15% water (based on wet crystal) at 50-80 deg.C for >=30min, preferably 30 min-48hr. When the above crystal is granule produced by granulator, the diameter of the granule is preferably 0.1-10.0mm.

公开(公告)号：JPS6333396A

公开(公告)日：1988-02-13

申请号：JP17556886

申请日：1986-07-28

Applicant: TOSOH CORP

Inventor： WAKAMATSU HIDETOSHI ,  IRINO SHIGETETSU ,  HARADA TSUNEO ,  TOKUDA AKIRA ,  KOYAMA KIYOTAKA

IPC: A23L27/30 ,  C07K1/00 ,  C07K5/072 ,  C07K5/075

Abstract: PURPOSE:To industrially and advantageously obtain the titled compound useful as a sweetener, etc., having improved solubility, by passing wet crystals of alpha-L-aspartyl-L-phenylalanine methyl ester through a region of specific water content at a specific temperature under normal pressure for drying. CONSTITUTION:Wet crystals of alpha-L-aspartyl-L-phenylalanine methyl ester (Aspartame) are subjected to solid-liquid separation with a centrifugal separator, passed through a screen, and granulated with a granulation machine. Then the granules are passed through a region of 5-15% based on the weight of wet crystals of alpha-L-aspartyl-L-phenylalanina methyl ester, water content at

公开(公告)号：JPS6317843A

公开(公告)日：1988-01-25

申请号：JP16335986

申请日：1986-07-11

Applicant: TOSOH CORP

Inventor： TAKAHASHI MITSURU ,  AKEYAMA HIDEO ,  KOYAMA KIYOTAKA

IPC: C07B61/00 ,  B01J23/06 ,  C07C51/00 ,  C07C51/15 ,  C07C57/52 ,  C07C67/00

Abstract: PURPOSE:To readily obtain the titled compound in high yield under mild reaction condition, by the presence of a specific cation in the reaction system in reacting a fluorine-containing halogenated alkene with carbon dioxide in the presence of zinc in an organic solvent. CONSTITUTION:A compound expressed by formula I [R1-R3 are H or alkyl and at least one thereof is F, fluorine-containing alkyl (particularly 1-20C perfluoro or polyfluoro aliphatic group having straight chain or branched chain); X is Cl, Br or I] is reacted with carbon dioxide in the presence of zinc which is subjected or not subjected to surface treatment to give a reaction product, which is then hydrolyzed to produce a compound expressed by formula II. In the process, one or more cations selected from alkali metal ions, alkaline earth metal ions or ammonium ions exist in the above-mentioned reaction system to suppress side reaction and readily provided the aimed compound in high yield.

公开(公告)号：JPH01163141A

公开(公告)日：1989-06-27

申请号：JP10417188

申请日：1988-04-28

Applicant: TOSOH CORP

Inventor： HIRONAKA TOSHIO ,  MIYAKE TAKANORI ,  SEKIZAWA KAZUHIKO ,  KOYAMA KIYOTAKA

IPC: C01B39/02 ,  B01J29/70 ,  C07B61/00 ,  C07C17/00 ,  C07C17/12 ,  C07C25/02 ,  C07C25/08 ,  C07C67/00

Abstract: PURPOSE:To obtain the aimed compound in high selectivity in producing the titled useful as a raw material for various organic compounds by chlorinating a benzene derivative in a liquid phase, by using a crystalline synthetic zeolite having a specific composition and structure as a catalyst. CONSTITUTION:In producing a para-substituted chlorinated benzene derivative such as para-dichlorobenzene useful as a raw material for drugs and agricultural chemicals by chlorinating a benzene derivative in a liquid phase, a crystalline synthetic zeolite which has a composition shown by the formula (M is one or more replaceable cations selected from groups I-VIII of the periodic table; n is valence of M; n is number of 0- about 6) in the expression of molar ratio of oxides and the substantially same X-ray diffraction pattern as that shown in the table is used as catalyst and the aimed compound is obtained in a high chlorine conversion ratio and in a higher selectivity, in higher yield and more stably than the well-known method while suppressing production of ortho- substituted derivative, metasubstituted derivative, polychlorinated derivative, chlorine adduct, etc., as by-products.

公开(公告)号：JPH01111894A

公开(公告)日：1989-04-28

申请号：JP26804987

申请日：1987-10-26

Applicant: TOSOH CORP

Inventor： HARADA TSUNEO ,  FUKUDA KENICHI ,  SHIMIZU HIROSHI ,  TOKUDA AKIRA ,  KOYAMA KIYOTAKA

IPC: C07K1/14 ,  C07K1/24 ,  C07K5/06 ,  C07K5/072 ,  C07K5/075 ,  C25B3/00 ,  C25B9/00 ,  C25B9/08 ,  C25D3/00

Abstract: PURPOSE:To efficiently remove org. acids with an anion-exchange membrane by supplying an aq. soln. of dipeptide ester(APM) contg. the org. acids into the intermediate chamber of an electrolytic cell, and electrolytically purifying the APM. CONSTITUTION:An aq. alpha-APM soln. contg. org. acids is supplied into the central section 7 of the electrolytic cell enclosed with an anion-exchange membrane 3 and a cation-exchange membrane 2 or plural anion-exchange membranes. When electrolysis is started, gaseous H2 is generated from a cathode 4, and gaseous chlorine is generated from an anode 5. The anions of the 1,3-benzyl-6- carboxymethyl-2,5-diketopiperazine(DKP), alpha-L-aspartyl-L-phenylalanine(AP), etc., are moved to an anode chamber 8 from the intermediate chamber 7, or the central chamber 7, through the anion-exchange membrane 3. The cations are moved to a cathode chamber 6. As a result, the inorg. ion and org. ion are efficiently removed.