公开(公告)号：JPS6219559A

公开(公告)日：1987-01-28

申请号：JP15836085

申请日：1985-07-19

Applicant: TORAY INDUSTRIES

Inventor： FURUYA MASAAKI ,  FUJINO TOSHIHIRO ,  NAKAOKA KENJI

IPC: C07C271/22

Abstract: PURPOSE:To obtain a compound useful as a synthetic raw material for peptides useful as medicines in high quality and at a low cost, by reacting D- or L-N - benzyloxycarbonyllysine with tert-butylphenyl carbonate. CONSTITUTION:D- or L-N -Benzyloxycarbonyllysine is reacted with tert- butylphenyl carbonate in the presence of an alkali metal compound in a polar organic solvent, e.g. dimethyl sulfoxide, at 50-100 deg.C for 1-8hr to afford the aimed substance. The reactin is carried out by using tert-butylphenyl carbonate in a molar amount of 1.0-1.5 times based on the D- or L-N - benzyloxycarbonyllysine, the solvent in an amount of 1.5-7 times based on the D- or L-N -benzyloxycarbonyllysine and the alkali metal compound in an amount of 1.0-1.2 equivalents based on the D- or L-N -benzyloxycarbonyllysine.

公开(公告)号：JPS54103870A

公开(公告)日：1979-08-15

申请号：JP1080578

申请日：1978-02-02

Applicant: TORAY INDUSTRIES

Inventor： SHIBAHARA TERUROU ,  FURUYA MASAAKI ,  IMAMURA SHINZOU

IPC: C07D235/28 ,  C08K5/34 ,  C08K5/36 ,  C23G1/06

Abstract: NEW MATERIAL:A 4,5,6,7-tetrahydrobenzimidazoline-2-thione derivative of formula I: (R is H, alkyl, allyl, or aralkyl group: R is alkyl, allyl, or aralkyl group). EXAMPLE:A compound of formula II. USE:Intermediate for medicines, chemicals for industrial rubbers, and their intermediates, and rust preventives. PROCESS:A 2-amino-cyclohexanone oxime or its derivative of formula III is reacted with a thiocyanate of formula IV, and the reaction product is treated with an acidic substance, e.g. bydrogen chloride to form the 4,5,6,7-tetrahydro-benzimidazoline- 2-thione derivative of formula I. The compound of formula II can be obtained by reacting cyclohexanone with NOCl and liquid SO2 to form a compound of formula V, which is reacted with a compound of the formula R NH2 in high yield industrially.

公开(公告)号：JPS6411630B2

公开(公告)日：1989-02-27

申请号：JP1080578

申请日：1978-02-02

Applicant: TORAY INDUSTRIES

Inventor： SHIBAHARA TETSURO ,  FURUYA MASAAKI ,  IMAMURA SHINZO

IPC: C07D235/28 ,  C08K5/34 ,  C08K5/36 ,  C23G1/06

公开(公告)号：JPS6032737A

公开(公告)日：1985-02-19

申请号：JP13763583

申请日：1983-07-29

Applicant: TORAY INDUSTRIES

Inventor： FURUYA MASAAKI ,  NAKAOKA KENJI

IPC: C07C29/124 ,  B01J27/00 ,  B01J27/232 ,  C07B61/00 ,  C07C27/00 ,  C07C33/26 ,  C07C67/00

Abstract: PURPOSE:To produce titled compound useful as a raw material of polyesters, resin additives, etc., in high purity, by hydrilyzing p-xylylen dichloride with a specific amount of water in the presence of an alkali metal (bi)carbonate. CONSTITUTION:p-xylylne dichloride is heated in 11-25 times weight of water base on p-xylylene dichloride in the presence of 1-1.3mol of an alkali metal carbonate or 2-2.5mol of an alkali metal bicarbonate based on 1mol of p- xylylene dichloride to obtain the objective compound in high purity suppressing the by-production of a benzyl ether-type dimer, oligomer, etc. The reaction is preferably carried out in the presence of a small amount of a hydrophobic organic solvent which is a good solvent of p-xylene dichloride and capable of forming an azeotropic mixture with water (e.g. toluene), thereby dissolving the p-xylylene dichloride crystal deposited at the upper part of the reactor by the reflux of the organic solvent, and preventing the deposition of the crystal.

公开(公告)号：JPS54106471A

公开(公告)日：1979-08-21

申请号：JP1147178

申请日：1978-02-06

Applicant: TORAY INDUSTRIES

Inventor： SHIBAHARA TERUROU ,  FURUYA MASAAKI ,  IMAMURA SHINZOU

IPC: C07D235/28

Abstract: PURPOSE:To obtain the title compound useful as an intermediate for medicines in high yield smoothly, by reacting a stable and easily available specific 2-aminocyclohexanone oxime or its salt with thiocyanic acid under specified conditions. CONSTITUTION:An 2-amino cyclohexanone oxime of formula I: (R is H, alkyl, allyl, or aralkyl group) or its salt is reacted with thiocyanic acid under neutral or acidic atmosphere (generally an acid, e.g. hydrochloric or sulfuric acid) in a solvent, e.g. water or (and) 1-8C alcohol at 40-180 deg.C, preferably 60-140 deg.C to give a 4, 5, 6, 7-tetrahydro-benzimidazoline-2-thione of formula II. The compound of formula I can be obtained by heating 2-chloro-1-nitroso-cyclohexane, prepared by reaction between cyclohexene and nitrosyl chloride, with liquid ammonia.