公开(公告)号：JPS63162661A

公开(公告)日：1988-07-06

申请号：JP30784386

申请日：1986-12-25

Applicant: SAGAMI CHEM RES

Inventor： FUCHIGAMI TAKAMASA ,  ISHII YOSHIMITSU ,  URATA HISAO

IPC: B01J31/20 ,  B01J31/00 ,  B01J31/24 ,  C07B61/00 ,  C07C67/00 ,  C07C231/00 ,  C07C231/10 ,  C07C233/04 ,  C07C233/05 ,  C07C233/06 ,  C07C233/08 ,  C07C233/11 ,  C07C233/65 ,  C07D295/18

Abstract: NEW MATERIAL:A compound shown by formula I (R and R are H, halogen or polyfluorocarbon; R -R are H, alkyl, aralkyl or aryl; R and R are H, alkyl or aralkyl). EXAMPLE:N,N-Diethyl-3-perfluorooctylpropanamide. USE:An intermediate for synthesizing fluorine-containing carboxylic acids useful as functional materials such as surface active agent, surface treatment, LB film, etc. PREPARATION:A fluorine-containing alkyl iodide shown by formula II is reacted with an amine shown by formula III and carbon monoxide in the presence of a cobalt or rhodium catalyst at 20-150 deg.C to give a compound shown by formula I. The amount of the catalyst used is 1/10,000-1/3 equivalent based on the compound shown by formula II. 1-Fluoro-3-iodopropane may be cited as the compound shown by formula II and diethylamine as the amine shown by formula III.

公开(公告)号：JPS63152344A

公开(公告)日：1988-06-24

申请号：JP22588286

申请日：1986-09-26

Applicant: SAGAMI CHEM RES

Inventor： FUCHIGAMI TAKAMASA ,  URATA HISAO ,  OBATA YOSHIKO

IPC: C07C67/38 ,  B01J23/42 ,  B01J23/44 ,  B01J27/10 ,  B01J27/13 ,  B01J27/185 ,  B01J31/24 ,  C07B61/00 ,  C07C67/347 ,  C07C69/63

Abstract: PURPOSE:To obtain the titled compound at a low cost, by reacting a polyfluoroalkyl iodide and an olefin compound each corresponding to the objective compound with alcohols and carbon monoxide in the presence of a group VIII transition metal catalyst and a base. CONSTITUTION:The objective compound of formula IV useful as a surfactant, etc., can be produced in high efficiency under a carbon monoxide partial pressure of and R are H, halogen or polyfluorocarbon residue) with (B) a compound of formula II (R -R are H, alkyl, aralkyl or aryl; R and R , R and R or R and R may together with bonded C atom form a ring; When R is not H, both R and R are not H at the same time), (C) a compound of formula III (R and R are group defined in R -R ; R and R may together with bonded C atom form a ring) and (D) carbon monoxide in the presence of (E) a group VIII transition metal catalyst (preferably palladium catalyst or platinum catalyst) and a base.

公开(公告)号：JPS63152343A

公开(公告)日：1988-06-24

申请号：JP22588186

申请日：1986-09-26

Applicant: SAGAMI CHEM RES

Inventor： FUCHIGAMI TAKAMASA ,  URATA HISAO ,  OBATA YOSHIKO

IPC: C07C67/38 ,  B01J27/10 ,  B01J31/20 ,  B01J31/22 ,  B01J31/24 ,  C07B61/00 ,  C07C67/347 ,  C07C69/65 ,  C07C69/653

Abstract: PURPOSE:To obtain the titled compound on an industrial scale at a low cost in one step, from a polyfluoroalkyl iodide and an acetylene compound each corresponding to the objective compound, by reacting the iodide and the acetylene compound with carbon monoxide and an alcohol in the presence of a palladium catalyst and a base. CONSTITUTION:The objective compound of formula III useful as an industrial raw material for a polymer having excellent stability, chemical resistance, weather resistance, water and oil repellency can be produced in one step from a raw material easily available on an industrial scale, by reacting (A) a compound of formula I (R and R are H, halogen or polyfluorocarbon residue), (B) a compound of formula R CidenticalCR (R and R are H, alkyl, aralkyl or aryl; when R is not H, R is not H), (C) carbon monoxide and (D) a compound of formula II (R and R are H, alkyl, aryl or aralkyl; R and R may together form a ring) in the presence of (E) a palladium catalyst and a base at 50-150 deg.C, preferably 60-100 deg.C.

公开(公告)号：JPS62228090A

公开(公告)日：1987-10-06

申请号：JP4168886

申请日：1986-02-28

Applicant: SAGAMI CHEM RES

Inventor： URATA HISAO ,  FUCHIGAMI TAKAMASA ,  TANAKA MARIKO ,  YAMADA KAORU ,  TOIDA NOBUKO

IPC: C07F15/00 ,  A61K31/505 ,  A61K31/555 ,  A61P35/00 ,  C07D239/54 ,  C07D239/553

Abstract: NEW MATERIAL:The compound of formula I (R and R are H, alkyl, alkenyl, aralkyl or O-containing heterocyclic group; M is Pd or Pt; X is halogen; L and L are unidentate ligand or together form a bidentate ligand). EXAMPLE:cis-( 2-Fluoro-3,5-dioxo-4, 6-dimethyl-4, 6-diaza-1-cyclohexenyl ) iodobis (triphenylphosphine)palladium. USE:An antitumor agent. PREPARATION:The objective compound can be produced e.g. according to the reaction formula by reacting the compound of formula II with the compound of formula III (n is 0-2 when L' is unidentate ligand and n is 0 or 1 when L' is bidentate ligand) in a solvent (usually benzene, etc.) at room temperature.

公开(公告)号：JPS62228069A

公开(公告)日：1987-10-06

申请号：JP11719686

申请日：1986-05-23

Applicant: SAGAMI CHEM RES

Inventor： FUCHIGAMI TAKAMASA ,  TANAKA MARIKO ,  YAMADA KAORU ,  TOIDA NOBUKO

IPC: C07D239/553 ,  A61K31/505 ,  A61P35/00 ,  C07D239/54

Abstract: NEW MATERIAL:A 1,3-disubstituted-5-fluoro-6-iodouracil derivative expressed by formula I (R and R are alkyl, alkenyl, aralkyl or oxygen-containing heterocyclic group). EXAMPLE:1,3-Dimethyl-5-fluoro-6-iodouracil. USE:An antitumor agent having improved toxicity of 5-fluorouracil and higher inhibition ratio of malignant tumor than that of 6-chloro derivatives. PREPARATION:A compound expressed by formula II is reacted in the presence of a base, e.g. butyllithium, lithium diisopropylamide, etc., preferably in an ether based solvent, e.g. diethyl ether, tetrahydrofuran, etc., to give a compound expressed by formula III, which is then reacted with an iodinating agent, e.g. iodine monochloride, iodine, etc., preferably in the above-mentioned solvent to afford the aimed compound expressed by formula I.

公开(公告)号：JPS6228932B2

公开(公告)日：1987-06-23

申请号：JP994083

申请日：1983-01-26

Applicant: SAGAMI CHEM RES

Inventor： OSHIMA IWAO ,  FUCHIGAMI TAKAMASA

IPC: C07C41/00 ,  B01J31/20 ,  C07C27/00 ,  C07C67/00

公开(公告)号：JPS6289642A

公开(公告)日：1987-04-24

申请号：JP22889885

申请日：1985-10-16

Applicant: SAGAMI CHEM RES

Inventor： FUCHIGAMI TAKAMASA ,  URATA HISAO ,  MURATA ATSUKO

IPC: C07C69/02 ,  C07C67/38 ,  C07C69/67

Abstract: NEW MATERIAL:A 3,3-diacyloxypropionic acid derivative expressed by formula I (R is lower alkyl; R is H or R CO). EXAMPLE:3,3-Dicetyloxypropionic acid acetic acid. USE:Useful as an intermediate capable of readily producing ethyl 3,3- diethoxypropionate or ethyl beta-ethoxyacrylate which is a synthetic intermediate for heterocyclic compounds, e.g. uracil, at a low cost. The compound expressed by formula I can be subjected to alcoholysis and readily converted into ethyl 3,3-diethoxypropionate, etc. PREPARATION:A carboxylic acid expressed by formula II is reacted with an olefin expressed by formula III, carbon monoxide and oxidizing agent, preferably oxygen in the presence of a palladium catalyst in the coexistence of a copper catalyst and/or alkali metal salt preferably by adding a carboxylic acid anhydride to afford the aimed compound expressed by formula I.

公开(公告)号：JPS6210498B2

公开(公告)日：1987-03-06

申请号：JP14048680

申请日：1980-10-09

Applicant: SAGAMI CHEM RES

Inventor： OSHIMA IWAO ,  FUCHIGAMI TAKAMASA

IPC: C07C69/653 ,  B01J31/00 ,  B01J31/16 ,  C07B61/00 ,  C07C27/00 ,  C07C29/14 ,  C07C33/46 ,  C07C45/00 ,  C07C45/50 ,  C07C47/24 ,  C07C67/00

公开(公告)号：JPS6191159A

公开(公告)日：1986-05-09

申请号：JP21056284

申请日：1984-10-09

Applicant: Sagami Chem Res Center ,  Toyo Soda Mfg Co Ltd

Inventor： HIRAI KENJI ,  FUJITA MAKOTO ,  FUCHIGAMI TAKAMASA

IPC: C07B61/00 ,  B01J23/00 ,  B01J23/40 ,  B01J23/74 ,  C07C227/08 ,  C07C229/36

CPC classification number: Y02P20/52

Abstract: PURPOSE: To produce the titled compound useful as a preparation raw material of food additives pharmaceuticals, etc., easily, in high yield and purity, by carrying out the reductive amination of phenylpyruvic acid restricting the amount of water existing in the solvent.
CONSTITUTION: The objective compound can be produced by reacting phenylpyruvic acid with an ammonia donor (e.g. ammonia water, ammonia gas, etc.) and hydrogen in an alcoholic solvent in the presence of a reduction catalyst (palladium supported by activated carbon, palladium black, etc.). The amount of water in the solvent is restricted to ≤30vol%, preferably 5W20% at the state of the reaction, and the reaction is carried out at room temperature W100°C. The amount of the ammonia donor is 1W15mol per 1mol of phenylpyruvic acid.
COPYRIGHT: (C)1986,JPO&Japio

Abstract translation: 目的：通过进行限制溶剂中存在的水量的苯基丙酮酸的还原胺化，以高产率和纯度容易地制备可用作食品添加剂药物等的制剂原料的标题化合物。 构成：目标化合物可以通过使苯基丙酮酸与氨供体（例如氨水，氨气等）和氢在醇溶剂中在还原催化剂（由活性炭负载的钯，钯黑， 等等。）。 在反应状态下，溶剂中的水的量限制在<30vol％，优选5-20％，反应在室温-100℃进行。 氨供体的量为每1mol苯基丙酮酸1-15mol。

公开(公告)号：JPS6094933A

公开(公告)日：1985-05-28

申请号：JP20273583

申请日：1983-10-31

Applicant: SAGAMI CHEM RES

Inventor： FUCHIGAMI TAKAMASA ,  SUZUKI YASUYUKI

IPC: C07C57/52 ,  B01J27/00 ,  B01J27/13 ,  B01J31/00 ,  B01J31/24 ,  B01J31/26 ,  C07B61/00 ,  C07C51/00 ,  C07C51/10 ,  C07C67/00

Abstract: PURPOSE:To produce the titled substance useful as a synthetic raw material for an anti-herpes agent, etc., in high yield, by reacting easily available 1-halo-1- perfluoroalkylethylene with water and CO in the presence of an iodine anion generating reagent, a base and a catalyst. CONSTITUTION:The objective compound of formula II can be produced by reacting the 1-halo-1-perfluoroalkylethylene of formula I (X is Cl or Br; Rf is 1-4C perfluoroalkyl) with water and carbon monoxide in the presence of an iodine anion generating reagent, a base such as pyridine and a palladium catalyst under normal or positive pressure at room temperature -150 deg.C. The iodine anion generating reagent is e.g. iodine, tetraethyl ammonium iodide, etc., and its amount is 0.5-10mol% based on the compound of formula I . The amount of the base is preferably 1-5 equivalent. The starting compound of formula I can be synthesized from a perfluoroalkylethylene.