公开(公告)号：DE69107579T2

公开(公告)日：1995-06-14

申请号：DE69107579

申请日：1991-11-15

Applicant: AGENCY IND SCIENCE TECHN

Inventor： YASUMOTO MASAHIKO ,  TSUCHIYA TOURU ,  SHIBUYA ISAO ,  YONEMOTO KATSUMI ,  TAGUCHI YOICHI C O NATIONAL CH

IPC: C07D285/34

Abstract: There is disclosed a method for producing 2,6-bis(disubstituted amino)-4-1,3,5-thiadiazine-4-one compounds represented by formula (I). The method comprises reacting an N,N-disubstituted cyanamide represented by formula (II) with carbonyl sulfide represented by formula (III) under a high pressure. wherein R1 and R2 each represent an alkyl group or R1 and R2 may bond together to form a ring, wherein R1 and R2 each have the same meanings as in formula (I), Formula (III> S = C = O . o

公开(公告)号：DE69107579D1

公开(公告)日：1995-03-30

申请号：DE69107579

申请日：1991-11-15

Applicant: AGENCY IND SCIENCE TECHN

Inventor： YASUMOTO MASAHIKO ,  TSUCHIYA TOURU ,  SHIBUYA ISAO ,  YONEMOTO KATSUMI ,  TAGUCHI YOICHI C O NATIONAL CH

IPC: C07D285/34

Abstract: There is disclosed a method for producing 2,6-bis(disubstituted amino)-4-1,3,5-thiadiazine-4-one compounds represented by formula (I). The method comprises reacting an N,N-disubstituted cyanamide represented by formula (II) with carbonyl sulfide represented by formula (III) under a high pressure. wherein R1 and R2 each represent an alkyl group or R1 and R2 may bond together to form a ring, wherein R1 and R2 each have the same meanings as in formula (I), Formula (III> S = C = O . o

公开(公告)号：JPH03261747A

公开(公告)日：1991-11-21

申请号：JP6080090

申请日：1990-03-12

Applicant: AGENCY IND SCIENCE TECHN

Inventor： YASUMOTO MASAHIKO ,  GOTO MIDORI ,  TSUCHIYA TORU ,  SHIBUYA ISAO

IPC: C07D295/02 ,  C07B43/04 ,  C07C209/22 ,  C07C211/63 ,  C07C211/64 ,  C07D213/20

Abstract: NEW MATERIAL:A thiocyanate of quaternary ammonium shown by formula I (R1 is alkyl or aralkyl; R2 to R4 are alkyl, aralkyl, aryl or mutually formed to give group as shown by formula II or formula III). EXAMPLE:Benzyltriethylammonium thiocyanate. USE:A surfactant, catalyst, drug and an intermediate thereof. PREPARATION:A thiocyanate shown by formula IV is reacted with a tertiary amine shown by formula V under normal pressure or high pressure to give a compound shown by formula I. By this method, the compound is obtained by using inexpensive raw materials by one stage in high yield.

公开(公告)号：JPS63221171A

公开(公告)日：1988-09-14

申请号：JP5479087

申请日：1987-03-10

Applicant: AGENCY IND SCIENCE TECHN

Inventor： YASUMOTO MASAHIKO ,  YANAGIYA KOSHIN ,  SHIBUYA ISAO ,  SEKIGUCHI TATSUO

IPC: C09B11/00 ,  C07C1/32 ,  C07C15/16 ,  C09B11/14

Abstract: PURPOSE:To obtain the title compd. which is a colorless crystal and has a high purity in a high yield without causing environmental pollution, by subjecting an arom. aldehyde and an arom. diamine to a dehydration-condensation reaction in the presence of optionally, a small amount of a reaction accelerator under high pressure. CONSTITUTION:An arom. aldehyde (A) such as benzaldehyde or a dialkylamino-, alkoxy-, alkyl-, NO2 or halogen-substd. benzaldehyde and an arom. amine (B) such as N,N-dialkylaniline, N-alkylaniline, aniline or a substitution compd. thereof are subjected to a dehydration-condensation reaction in the presence of a optionally, 0.1-50mol.% (based on the amount of the component A) of a reaction accelerator such as protonic acid, Lewis acid, etc. under a high pressure of 1,000-9,000kg/cm .

公开(公告)号：JPH01230674A

公开(公告)日：1989-09-14

申请号：JP5912688

申请日：1988-03-11

Applicant: AGENCY IND SCIENCE TECHN

Inventor： TANAKA MOTOO ,  SEKIGUCHI TATSUO ,  KAWABATA KOJIRO ,  NAKAMURA TAKAYOSHI ,  TACHIBANA HIROAKI ,  MANDA EIICHIRO ,  YASUMOTO MASAHIKO ,  SHIBUYA ISAO

IPC: B41M5/26 ,  C09B23/00 ,  C09B57/00 ,  G03G5/06

Abstract: PURPOSE:To obtain a high-purity squarylium pigment suitable as, e.g., a recording material for optical discs is high yields, by condensing a specified colorant intermediate through dehydration with squaric acid in an organic solvent under a pressure higher than a specified value. CONSTITUTION:A colorant intermediate of the general formula R-H [wherein R is formula I, II, III or IV, R is C18H37, R is H, CH3 or Cl, R is CH3, R is H or CH3, R is H or Cl, X is C(CH3)2, Se or S, and Y is p- chlorobenzenesulfonic acid], e.g., (2,3,3-trimethyl-1-octadecyl-indolinium) p- chlorobenzenesulfonate, is condensed through dehydration with squaric acid in an organic solvent (e.g., methanol) under a high pressure >=1000kg/cm to obtain a squarylium colorant of formula V.

公开(公告)号：JPS63218673A

公开(公告)日：1988-09-12

申请号：JP5370187

申请日：1987-03-09

Applicant: AGENCY IND SCIENCE TECHN

Inventor： SHIBUYA ISAO ,  YANAGIYA KOSHIN ,  YASUMOTO MASAHIKO

IPC: C07D339/06 ,  B01J31/02 ,  C07B61/00 ,  C07D409/04

Abstract: PURPOSE:To obtain the titled compound which is an intermediate for synthetic compound such as medicine in one process and high yield without by-product, by using an acetylene compound, carbon disulfide and sulfur which are simple raw material and reacting the acetylene compound with the carbon disulfide and sulfur under high pressure in the presence of a base. CONSTITUTION:Acetylenes expressed by formula I (R and R are inert substituent groups or H), carbon disulfide and sulfur are used as raw material and the acetylenes are reacted with the carbon disulfide and sulfur under high pressure in the presence of a base, preferably triethylamine, pyridine, N,N- dimethylaniline, etc., preferably at room temperature - 100 deg.C normally for 5-50hr to provided the aimed compound expressed by formula II. Commercial products may be directly use as the carbon disulfide and sulfur which are the above-mentioned raw material and the carbon disulfide is preferably used in excess amount, since the carbon disulfide is a raw material for dissolving sulfur. Although higher pressure is preferred, the pressure is suitable normally in the range of 500-9,000kg/cm .

公开(公告)号：JPH04182475A

公开(公告)日：1992-06-30

申请号：JP30925090

申请日：1990-11-15

Applicant: AGENCY IND SCIENCE TECHN

Inventor： YASUMOTO MASAHIKO ,  TSUCHIYA TORU ,  TAGUCHI YOICHI ,  SHIBUYA ISAO ,  YONEMOTO KATSUMI

IPC: C07D285/34

Abstract: PURPOSE:To obtain a compound useful as an intermediate for medicine or agricultural chemical in one-stage reaction and good yield from an inexpensive raw material by reacting an N,N-disubstituted-cyanamide with carbonylsulfide under high pressure. CONSTITUTION:A N,N-di-substituted cyanamide expressed by formula I (R1 and R2 are alkyl or R1 and R2 may together form a ring) is reacted with carbonyl sulfide expressed by the formula S=C=O in a solvent such as toluene at 20-200 deg.C under pressure of 1000-12000 atom to provide the objective product expressed by formula II. The compound expressed by formula I and carbonyl sulfide are used at a molar ratio of 1:10 to 10:1. The compound expressed by formula II is used as an intermediate for drug for inflammatory disease and cardiopathy and useful as an intermediate for nematocide, insect pest control agent, etc.

公开(公告)号：JPH03264595A

公开(公告)日：1991-11-25

申请号：JP6206690

申请日：1990-03-13

Applicant: AGENCY IND SCIENCE TECHN

Inventor： SASAKI MAKOTO ,  GAMA YASUO ,  YASUMOTO MASAHIKO ,  ISHIGAMI YUTAKA

IPC: C07H1/00 ,  C07H15/04 ,  C07H15/18 ,  C07H15/203 ,  C07J17/00

Abstract: PURPOSE:To simply, safely, economically and highly selectively prepare a glycosylated compound by reacting a halogenated saccharide derivative with an alcohol in the presence of a tertial amine under a high pressure. CONSTITUTION:1.2-1.5 Equivalent (based on an alcohol) of a halogenated saccharide derivative (OH and amino groups are preliminarily protected with protecting groups) such as glucopyranosyl bromide, the alcohol such as methanol and molecular sieve 4A are dissolved in a solvent such as methylene chloride, sealed in a Teflon capsule, set in a high pressure reactor and subsequently subjected to a reaction at room temperature to 40 deg.C for 20-40 hours under >=4000 atmospheric pressure to form the objective glycosylation product, which is recrystallized, etc.

公开(公告)号：JPS61189273A

公开(公告)日：1986-08-22

申请号：JP3089385

申请日：1985-02-19

Applicant: AGENCY IND SCIENCE TECHN

Inventor： YASUMOTO MASAHIKO ,  YANAGIYA KOSHIN ,  KURABAYASHI MASAHIRO

IPC: C07D409/04 ,  C07D213/00 ,  C07D235/00 ,  C07D235/06 ,  C07D307/00 ,  C07D333/00 ,  C07D401/04 ,  C07D405/04

Abstract: PURPOSE:To obtain the titled substance useful as pharmaceuticals, agricultural chemicals, etc. on one step, in high yield, without using a reaction reagent which might cause the environmental pollution, from inexpensive raw materials, by reacting a nitrile with o-phenylenediamine in the presence of an alcohol under pressure. CONSTITUTION:The compound of formula III is produced by reacting the nitrile of formula I (R1 is alkyl, aryl, aralkyl or heterocyclic group which may have substituent group) with the o-phenylenediamine of formula II (R2 is same as R1 or H, halogen, nitro or N-substituted amino) in the presence of an alcohol under high pressure (higher the better; usually 1,000-9,000kg/cm ) at 30-150 deg.C. The molar ratio of the nitrile of formula I to the compound of formula II is preferably 1:5-5:1, and the amount of the alcohol is 0.1-10mol per 1mol of the nitrile.

公开(公告)号：JP2000265198A

公开(公告)日：2000-09-26

申请号：JP7079499

申请日：1999-03-16

Applicant: AGENCY IND SCIENCE TECHN ,  RES INST INNOVATIVE TECH EARTH

Inventor： NICHIAKI TOSHIHIKO ,  MURATA JUNJI ,  YASUMOTO MASAHIKO ,  SAKO TAKESHI ,  SEKIYA AKIRA

IPC: C11D7/50 ,  C09D7/12 ,  C09K5/04

Abstract: PROBLEM TO BE SOLVED: To prepare an azeotropic or azeotropic-like composition not causing ozone depletion, sparingly having greenhouse effect and toxicity, excellent in detergency and useful for a detergent for electronic parts and optical lens or the like by including bistrifluoreoethyl ether and propanol. SOLUTION: This composition consists of (A) (preferably 85-95 mol%, more preferably 89.0 mol%) bis(2,2,2-trifluoroethyl)ether expressed by the formula CF3CH2OCH2CF3 and (B) (preferably 5-15 mol%, more preferably 11.0 mol%) 1-propanol. The composition is preferably formulated with 0.1-5 wt.% stabilizer such as nitromethane and 0.3-5 wt.% surfactant such as a nonionic surfactant, a cationic one or an anionic one.