公开(公告)号：JPH0892195A

公开(公告)日：1996-04-09

申请号：JP23159694

申请日：1994-09-27

Applicant: MITSUI TOATSU CHEMICALS

Inventor： NAKATSUKA MASAKATSU ,  UMEDA SHINICHI ,  TAKAOKA MASAZUMI ,  MIZUTA HIDEKI ,  NAGATA TERUYUKI

IPC: B41M5/333 ,  B41M5/30 ,  C07C269/04 ,  C07C271/28 ,  C07C271/38 ,  C07C271/58 ,  C07C333/08 ,  C07C333/24 ,  C09K9/02

Abstract: PURPOSE: To produce a carbamate-substituted salicylic acid derivative having high purity in a high yield and shortened time by reacting a specific aminosalicylic acid derivative with a specific haloformate compound in the presence of a trialkylamine. CONSTITUTION: A salicylic acid derivative of formula III is produced by reacting (A) a compound of formula I (X1 and X2 are each H, an alkyl, an alkoxy, an aralkyl, an aryl or a halogen; R1 is H, an alkyl, an aralkyl or an aryl) with (B) a compound of formula II (Y1 and Y2 are each O or S; R2 is an alkyl, an alkenyl, an aralkyl or an aryl; Z is a halogen) in the presence of a trialkylamine. An example of the salicylic acid derivative is 4-(n- octyloxycarbonylamino)salicylic acid. The derivative is useful as an electron accepting compound (color developing agent) for recording materials such as pressure-sensitive or heat-sensitive recording materials, etc.

公开(公告)号：JPH0892173A

公开(公告)日：1996-04-09

申请号：JP23509794

申请日：1994-09-29

Applicant: MITSUI TOATSU CHEMICALS

Inventor： MIZUTA HIDEKI ,  TAKAOKA MASAZUMI ,  NARUSE HIROSHI ,  NAGATA TERUYUKI

IPC: C07C209/08 ,  C07C209/84 ,  C07C211/10

Abstract: PURPOSE: To isolate the high-quality compound useful as a raw material or an intermediate for medicines and industrial chemicals in a high yield by extracting a reacted liquid of a dihalogenoethane with an alkylamine in the presence of a basic compound using an extracting solvent. CONSTITUTION: This method for producing N,N'-dialkylethylenediamine (preferably N,N'-dimethylethylenediamine) of the formula is to react (A) a 1,2- dihalogenoethane (especially preferably 1,2-dichloroethane) with (B) an alkyldiamine (preferably a liquid) of the formula R-NH2 (R is a 1-2C alkyl)and carry out salting out and extraction of the resultant reacted liquid using (D) an extracting solvent (a solvent which is immiscible with water and does not make azeotropic mixture with the product, preferably benzene) in the presence of (C) a basic compound (especially preferably a saturated aqueous solution of sodium hydroxide).

公开(公告)号：JPH04316571A

公开(公告)日：1992-11-06

申请号：JP8372291

申请日：1991-04-16

Applicant: MITSUI TOATSU CHEMICALS

Inventor： KAMASHITA TOMOKO ,  TAKAOKA MASAZUMI ,  WADA MASARU ,  NAGATA TERUYUKI

IPC: B01J31/02 ,  C07B61/00 ,  C07D307/66

Abstract: PURPOSE:To obtain the subject compound useful as an intermediate for amino acid ester, intermediate for peptide synthesis and raw material for sweetener by reacting an N-protected aspartic acid with phosgene in the presence of a lower aliphatic amide catalyst while supplying the phosgene to the system under specific condition. CONSTITUTION:The objective compound can be produced by reacting an N- protected aspartic acid (e.g. N-benzyloxycarbonyl-L-aspartic acid) in an inert organic solvent (e.g. chlorobenzene) in the presence of a lower aliphatic amide catalyst (e.g. dimethylformamide) while blowing phosgene and an inert gas into the solvent. In the above process, phosgene is supplied at a rate to keep the reaction mass in a state essentially free from residual unreacted phosgene until the reaction approaches the end point.

公开(公告)号：JPH0892194A

公开(公告)日：1996-04-09

申请号：JP23159594

申请日：1994-09-27

Applicant: MITSUI TOATSU CHEMICALS

Inventor： NAKATSUKA MASAKATSU ,  UMEDA SHINICHI ,  TAKAOKA MASAZUMI ,  MIZUTA HIDEKI ,  NAGATA TERUYUKI

IPC: B41M5/333 ,  B41M5/30 ,  C07C269/04 ,  C07C271/28 ,  C07C271/38 ,  C07C271/58 ,  C07C333/08 ,  C07C333/24 ,  C09K9/02

Abstract: PURPOSE: To produce a carbamate-substituted salicylic acid derivative having high purity in a high yield by reacting a specific alkali metal salt of an aminosalicylic acid derivative with a specific haloformate compound in an alcoholic solvent. CONSTITUTION: A salicylic acid derivative of formula III is produced by reacting (A) an alkali metal salt of a compound of formula I (X1 and X2 are each H, an alkyl, an alkoxy, an aralkyl, an aryl or a halogen; R1 is H, an alkyl, an aralkyl or an aryl) with (B) a compound of formula II (Y1 and Y2 are each O or S; R2 ), is an alkyl, an alkenyl, an aralkyl or an aryl; Z is a halogen) in an alcoholic solvent. An example of the salicylic acid derivative is 4-(n- octyloxycarbonylamino)salicylic acid. The derivative is useful as an electron accepting compound (color developing agent) for recording materials such as heat-sensitive or pressure-sensitive recording materials, etc.

公开(公告)号：JPH07165650A

公开(公告)日：1995-06-27

申请号：JP31699193

申请日：1993-12-16

Applicant: MITSUI TOATSU CHEMICALS

Inventor： MIZUTA HIDEKI ,  TAKAOKA MASAZUMI ,  NAGATA TERUYUKI

IPC: B01J23/44 ,  B01J23/74 ,  C07B61/00 ,  C07C37/20 ,  C07C37/70 ,  C07C39/07

Abstract: PURPOSE:To industrially obtain 2,4-xylenol in high yield and purity which have never been attained by conventional techniques. CONSTITUTION:This high-purity 2,4-xylenol is obtained by hydrogenolysis of a mixture of 2-N,N-dialkylaminomethyl-4methylphenol and 2,6-di(N,N- dialkylaminomethyl)-4-methylphenol produced by reaction between p-cresol, formaldehyde and a secondary amine. In this process, hydrogen feed during the hydrogenolysis is discontinued arbitrarily.

公开(公告)号：JPH07165649A

公开(公告)日：1995-06-27

申请号：JP31699093

申请日：1993-12-16

Applicant: MITSUI TOATSU CHEMICALS

Inventor： MIZUTA HIDEKI ,  TAKAOKA MASAZUMI ,  NAGATA TERUYUKI

IPC: B01J23/40 ,  B01J23/74 ,  C07B61/00 ,  C07C37/00 ,  C07C37/70 ,  C07C39/06

Abstract: PURPOSE:To efficiently obtain an alkylated phenol useful as e.g. an industrial chemical in high yield, by hydrogenolysis of a specific aminoalkylated phenol under specified conditions. CONSTITUTION:This alkylated phenol of formula II (R' is a lower alkyl; (m) is 1-3) is obtained by hydrogenolysis of an aminoalkylated phenol produced from a phenol compound of formula I (R is H or a lower alkyl; (n) is 0-2) (e.g. a cresol), an aliphatic aldehyde such as formaldehyde and a secondary amine such as dimethylamine while drawing the secondary amine produced during the hydrogenolysis out of the system. It is preferable that the temperature in the hydrogenolysis be at or higher than the dissociation temperature of the secondary amine salt of the alkylated phenol but not higher than the boiling point of the alkylated phenol.

公开(公告)号：JPH04316570A

公开(公告)日：1992-11-06

申请号：JP8371391

申请日：1991-04-16

Applicant: MITSUI TOATSU CHEMICALS

Inventor： KAMASHITA TOMOKO ,  TAKAOKA MASAZUMI ,  WADA MASARU ,  NAGATA TERUYUKI

IPC: C07B61/00 ,  C07D307/66

Abstract: PURPOSE:To obtain the subject compound useful as a raw material for sweetener, etc., in high yield and purity by reacting an N-protected aspartic acid in an inert organic solvent in the presence of a catalyst while blowing phosgene and an inert gas into the solvent. CONSTITUTION:The objective N-protected aspartic acid anhydride is produced by reacting an N-protected aspartic acid in an inert organic solvent in the presence of a catalyst while blowing phosgene and an inert gas into the solvent. The N-protecting group is formyl, acetyl, trifluoroacetyl, etc., and the inert gas is dry air, nitrogen, argon, etc.