公开(公告)号：JPH10249186A

公开(公告)日：1998-09-22

申请号：JP6277397

申请日：1997-03-17

Applicant: AGENCY IND SCIENCE TECHN

Inventor： SHIMADA SATORU ,  TAKEDA HIROYUKI ,  ONISHI SATOMI ,  NAKANISHI FUSAE ,  MATSUDA HIROO

IPC: G03C1/73 ,  B01J19/00 ,  C23C30/00

Abstract: PROBLEM TO BE SOLVED: To impart reactivity to the ethynyl group part of an asymmetric disulfide compd. by adsorbing the disulfide compd. on the surface of gold. SOLUTION: The disulfide compd. is represented by the formula (where Ar is aryl that may have a substituent, e.g. phenyl, tolyl, xylyl, naphthyl or methylnaphthyl and the substituent is, e.g. alkoxy having about 1-6C, preferably about 1-4C lower alkyl, hydroxyl, amino or phenylethynyl). The disulfide compd. is adsorbed on the surface of gold by bringing a soln. contg. the disulfide compd. into contact with the surface of the gold. A method for dipping the gold in the soln. may be adopted as the contact method.

公开(公告)号：JPH11100385A

公开(公告)日：1999-04-13

申请号：JP26459797

申请日：1997-09-29

Applicant: AGENCY IND SCIENCE TECHN ,  SHIMADA SATORU ,  ONISHI SATOMI ,  MATSUDA HIROO ,  NAKANISHI FUSAE

Inventor： SHIMADA SATORU ,  ONISHI SATOMI ,  MATSUDA HIROO ,  NAKANISHI FUSAE ,  TAKEDA HIROYUKI

IPC: G02F1/35 ,  C07F1/12 ,  C07F7/08 ,  C23C22/00 ,  G02B1/00 ,  G02B1/04 ,  G02F1/355 ,  G11B7/244

Abstract: PROBLEM TO BE SOLVED: To obtain gold with an adsorbed unimolecular layer of an organic thio group, useful as a nonlinear optical material by bringing the gold into contact with a specific solution in the presence of fluoride ion. SOLUTION: This gold with an adsorbed unimolecular layer of an organic thio group is the gold having the organic thio group of formula I or II [R , R , R and R are each an aryl or an (un)saturated aliphatic group] on the surface thereof adsorbed so as to form the unimolecular layer, and obtained by bringing the gold into contact with a solution containing tri(lower alkyl) silylethyl sulfide of formula III [R is an aryl or an (un)saturated apliphatic group] in the presence of fluoride ion. For example, a quarternary ammonium salt and hydrofluoric acid, especially tetrabutylammonium fluoride, are used as a fluoride ion source.

公开(公告)号：JPH0948848A

公开(公告)日：1997-02-18

申请号：JP19958495

申请日：1995-08-04

Applicant: AGENCY IND SCIENCE TECHN

Inventor： TAMAOKI NOBUYUKI ,  SHIMADA SATORU

IPC: C08G69/00 ,  C08G69/26 ,  C08G69/28

Abstract: PROBLEM TO BE SOLVED: To obtain the subject polymer for rubbers not losing their elasticity at extremely low temperatures in the space, etc., in a good yield by using a bifunctional monomer capable of polycondensing or addition-polymerizing with the functional groups of a bifunctional catenane having a specific structure as connection units. SOLUTION: (A) A bifunctional catenane [2] whose two cyclic units have amino groups, respectively, is polycondensed with (B) adipic acid dichloride. For example, 10-aza-hexaethylene glycol having a protected amino group is cyclized with 2,4-bis-(4-hydroxyphenyl)-1,10-diazaphenanthroline by the method of Sovaju et al., and the protecting group is subsequently removed from the product to give the bifunctional catenane [2]. The obtained catenane [2] is polymerized with adipic dichloride in the presence of triethylamine in methylene dichloride at room temperature to give the polymer. The catenane [2] of the interlock units and the connection units are preferably used in a reaction molar ratio of 1:1.

公开(公告)号：JPH09227552A

公开(公告)日：1997-09-02

申请号：JP4274896

申请日：1996-02-29

Applicant: AGENCY IND SCIENCE TECHN

Inventor： SHIMADA SATORU ,  MATSUDA HIROO ,  OKADA SHUJI ,  NAKANISHI HACHIRO

IPC: G03C1/73 ,  C07D339/06 ,  C08F38/02 ,  G02B1/04

Abstract: PROBLEM TO BE SOLVED: To obtain a new compound useful as a raw material for a functional material such as nonlinear optical material, photosensitive material, polymer semiconductor crystal, etc., having solid-phase polymerizability. SOLUTION: This diacetylene derivative is shown by formula I (Ar is a bifunctional aromatic group; (m) and (n) are each 2-12). The compound of formula I is obtained by reacting a 1,3-alkadiynecarboxylic acid amide compound of the formula, CH3 -(CH2 )m-C≡C-C≡C-(CH2 )n -CONH-Ar-COOH or its acid halide with hydroxymethyltetrathiafulvalene of formula II in an inert gas atmosphere (e.g. nitrogen gas) in a solvent (e.g. methylene chloride) at 0-50 deg.C. The 1,3-alkadiynecarboxylic acid amide compound is obtained by reacting an 1,3- alkadiynecarboxylic acid compound of the formula, CH3 -(CH2 )m - C≡C-C≡C-(CH2 )n -COOR (R is H or a halogen) with an aromatic aminocarboxylic acid ester of the formula, H2 N-Ar-COOR (R is a hydrocarbon) and hydrolyzing the ester bond.

公开(公告)号：JPH0948849A

公开(公告)日：1997-02-18

申请号：JP19958795

申请日：1995-08-04

Applicant: AGENCY IND SCIENCE TECHN

Inventor： SHIMADA SATORU ,  TAMAOKI NOBUYUKI ,  ISHIKAWA KEIICHIRO

IPC: C08G69/00 ,  C08G69/26

Abstract: PROBLEM TO BE SOLVED: To obtain the subject polymer composed from a monomer having an interlock structure, not having a chemical bond between the repeating units, and useful as a raw material for functional materials such as polymer elastomers, etc. SOLUTION: An interlock polymer comprises a 2-catenane derivative of formula I (n is an integer of 0-2; X is an integer). The compound of formula I is obtained e.g. by reacting a 2-catenane derivative of formula II as a starting raw material with copper borofluoride, reacting the copper ion-introduced product with adipic dichloride and subsequently reacting the obtained compound with a cyanide ion to remove the copper ion. The bifunctional 2-catenane of formula II is obtained e.g. by cyclizing an amino-protected 10-aza-hexaethylene glycol with 2,4-bis-(4-hydroxyphenyl)-1,10-diazaphenanthroline by the method of Sovaju et al. and subsequently removing the protecting group from the product.

公开(公告)号：JPH07233141A

公开(公告)日：1995-09-05

申请号：JP5133894

申请日：1994-02-23

Applicant: AGENCY IND SCIENCE TECHN

Inventor： SHIMADA SATORU ,  MATSUDA HIROO ,  MINAMI SHINJI ,  OKADA SHUJI ,  NAKANISHI HACHIRO

IPC: C07C319/18 ,  C07C319/14 ,  C07C323/19

Abstract: PURPOSE:To obtain a diacetylene derivative which has an S atom directly bonded to a C atom in the triple bond and shows a large electronic effect and solid-phase polymerizability, thus is useful as a functional material such as a nonlinear optical material, a photosensitive material and a polymer semiconductor crystal. CONSTITUTION:The compound of formula I [Ar , Ar are (substituted) phenyl; n is 1-8], for example, 8-(4-bromophenyl)thio-5,7-octadiynyl phenylcarbamate. The compound of formula I is prepared by protecting the terminal hydroxy group in omega-hydroxy-1,3-alkadiyne of formula II, introducing an arylthio group into the 1-position of the protected omega-hydroxy-1,3-alkadiyne, deprotecting the product of the diacetylene derivative of formula III and allowing the deprotected hydroxyl to react with an aryl isocyanate to effect introduction of a urethane group on the chain terminal.

公开(公告)号：JPH11255757A

公开(公告)日：1999-09-21

申请号：JP5536598

申请日：1998-03-06

Applicant: AGENCY IND SCIENCE TECHN ,  SHIMADA SATORU ,  MATSUDA HIROO

Inventor： SHIMADA SATORU ,  MATSUDA HIROO ,  OKADA SHUJI ,  NAKANISHI HACHIRO

IPC: C07D273/01 ,  G02F1/35 ,  G02F1/355 ,  G02F1/361

Abstract: PROBLEM TO BE SOLVED: To obtain the subject new compound having crown ether structure, high in ion transfer ability, capable of solid phase polymerization, and useful as a raw material for functional materials such as electroconductive materials, electrode materials, nonlinear optical materials, photosensitive materials and semiconductor crystals. SOLUTION: This new compound is shown by the formula CH3 -(CH2 )k -C≡C- C≡C-(CH2 )m -CO- E [(k) and (m) are each 1-12; E is a structure of the formula ((n) is 1-4)], e.g. CH3 -(CH2 )11 -C≡C-C≡C-(CH2 )8 -COOH. This new compound of the above formula is obtained by reaction of a 1,3-alkadiynecarboxylic acid compound of the formula CH3 -(CH2 )k -C≡C-C≡C-(CH2 )m -COX (X is hydroxyl or a halogen) with an azacrown compound of the formula H-E pref. at 1.1-1.2 mol per mol of the 1,3-alkadiynecarboxylic acid compound in an aprotic solvent (e.g. methylene chloride, an ether compound) in an inert gas atmosphere such as argon or nitrogen under normal pressures pref. at 25-40 deg.C under agitation.

公开(公告)号：JPH11100386A

公开(公告)日：1999-04-13

申请号：JP26457397

申请日：1997-09-29

Applicant: AGENCY IND SCIENCE TECHN ,  SHIMADA SATORU ,  ONISHI SATOMI ,  MATSUDA HIROO ,  NAKANISHI FUSAE

Inventor： SHIMADA SATORU ,  ONISHI SATOMI ,  MATSUDA HIROO ,  NAKANISHI FUSAE ,  TAKEDA HIROYUKI

IPC: C07F7/08

Abstract: PROBLEM TO BE SOLVED: To obtain a sulfide compound useful as a nonlinear optical material or the like and usable as a stable thiol equivalent by reacting a specific compound with an organic metal compound. SOLUTION: This sulfide compound is a compound of formulas I to III [R , R , R and R are each an aryl or an (un)saturated aliphatic group; R is a lower alkyl; Ar is an aryl], e.g. (trimethylsilylethyl)phenylacetylene sulfide. The compound is obtained by reacting a tri(lower alkyl)silylethylsulfenyl compound of formula IV (X is a halogen or p-toluenesulfonyl) with an organic metal compound of formula V or VI [M is an alkali(alkaline earth) metal] or the formula R -M (R is the same as R or the like).