公开(公告)号：JPH0597781A

公开(公告)日：1993-04-20

申请号：JP27897291

申请日：1991-10-01

Applicant: MITSUI PETROCHEMICAL IND

Inventor： OYOSHI HAJIME ,  KONDO MASAHIRO ,  TARUMOTO HIROMASA ,  TANAKA MICHIO

IPC: C07C213/02 ,  C07C215/76

Abstract: PURPOSE:To obtain the subject compound useful as an intermediate for agricultural chemicals in high selectivity and yield without causing corrosion of a reactor by reacting specific aminophenols with dialkyl sulfate under specified conditions. CONSTITUTION:Aminophenols such as o-aminophenol expressed by formula I (R is H or alkyl) are reacted with a dialkyl sulfate such as dimethyl sulfate at 30-70 deg.C to provide the objective compound of formula II (R is alkyl). Furthermore, the dialkyl sulfate is preferably used in an amount of 1.0-1.2mol, based on 1mol compound of formula I.

公开(公告)号：JPS63162643A

公开(公告)日：1988-07-06

申请号：JP31110786

申请日：1986-12-25

Applicant: MITSUI PETROCHEMICAL IND

Inventor： ONO NORIO ,  MATSUOKA HIDETO ,  TARUMOTO HIROMASA

IPC: C07C43/295 ,  C07C41/00 ,  C07C41/38 ,  C07C41/40 ,  C07C67/00

Abstract: PURPOSE:To separate the titled compound efficiently, by dehydrating dimerizing hydroquinone in a water-immiscible solvent to give a reaction mixture and adding a blend of water and one or more selected from an alkyl ether, a dialkyl ketone, a carboxylic acid ester, etc., to the reaction mixture. CONSTITUTION:In obtaining 4,4'-dihydroxydiphenyl ether by dehydrating and dimerizing hydroquinone, the reaction is carried out by using a water-immiscible solvent such as mesitylene, xylene, toluene, cumene, etc. A liquid reaction mixture, obtained afterward, containing unreacted hydroquinone is incorporated with a blend of water and one or more selected from a group consisting of an alkyl ether, a dialkyl ketone, a carboxylic acid ester, >=4C aliphatic alcohol, a nitrile and a halogenated hydrocarbon into two liquid phases of a water phase and an oil phase, which are separated and the titled compound useful as a raw material for synthetic polymers and organic chemicals is obtained from the oil phase.

公开(公告)号：JPH02202873A

公开(公告)日：1990-08-10

申请号：JP2449089

申请日：1989-02-01

Applicant: MITSUI PETROCHEMICAL IND

Inventor： HIROWATARI NORIYUKI ,  KURANO YOSHITO ,  TARUMOTO HIROMASA ,  FURUYA YOSHIRO

IPC: C07D211/92

Abstract: PURPOSE:To easily produce the subject compound in high yield and purity at about normal temperature by reducing 2,2,6,6-tetraalkyl-4-piperidinone with hydrogen in a solvent in the presence of a catalyst, removing by-products and adding a halogen to the product in the presence of an alkali. CONSTITUTION:The objective compound useful as a component of bleaching detergent, etc., can be produced by (1) reducing 2,2,6,6-tetraalkyl-4-piperidinone with hydrogen in an aqueous solvent in the presence of a catalyst (e.g. Raney nickel) under hydrogen pressure of 6-20kg/cm C at 30-100 deg.C for 1-12hr to form 2,2,6,6-tetraalkyl-4-piperidinol, (2) separating the catalyst by filtration and the low-boiling by products by distillation, (3) extracting with an organic solvent inert to the following halogenation reaction, (4) adding a halogen such as Cl2 to the reaction mixture containing 2,2,6,6-tetraalkyl-4-piperazinol in the presence of an alkali and (5) reacting at 0-60 deg.C under a pressure of 1-10kg/cm for 1-20hr.

公开(公告)号：JPH02145571A

公开(公告)日：1990-06-05

申请号：JP30031588

申请日：1988-11-28

Applicant: MITSUI PETROCHEMICAL IND

Inventor： HIROWATARI NORIYUKI ,  TARUMOTO HIROMASA ,  KONDO MASAHIRO ,  FURUYA YOSHIRO

IPC: C07D211/74 ,  B01J27/24 ,  C07B61/00

Abstract: PURPOSE:To obtain the subject compound in high yield in a short time by two-stage reaction comprising the 1st-stage reaction to introduce ammonia into acetones in the presence of a catalyst under a specific condition and the 2nd-stage reaction to perform the reaction at a specific temperature without introducing ammonia or adding acetones to the system. CONSTITUTION:The subject compound useful as a raw material for polymer stabilizer or bleaching agent, etc., is produced in a short time in high yield with a two-stage reaction having easily controllable temperature by (1) introducing ammonia into acetone and/or its condensate (acetones) in the presence of a catalyst (preferably protonic acid or its ammonium salt) at a molar ratio (acetone/ammonia) of 3-10 (preferably 4-6) and reacting at 45-55 deg.C under introduction of ammonia and (2) stopping the introduction of ammonia and successively reacting the components at 55-70 deg.C (higher than the temperature of the 1st stage reaction) without separating and purifying the produced acetone nor adding additional acetones to the system.

公开(公告)号：JPH0112737B2

公开(公告)日：1989-03-02

申请号：JP3177882

申请日：1982-03-02

Applicant: MITSUI PETROCHEMICAL IND

Inventor： NAKAGAWA HIROAKI ,  MIZUNO KENICHI ,  MATSUMOTO TETSUHIRO ,  TARUMOTO HIROMASA

IPC: C07C37/08 ,  B01J27/02 ,  C07B61/00 ,  C07C27/00 ,  C07C39/10 ,  C07C67/00

公开(公告)号：JPH051072A

公开(公告)日：1993-01-08

申请号：JP10448491

申请日：1991-05-09

Applicant: MITSUI PETROCHEMICAL IND

Inventor： TANAKA MICHIO ,  TARUMOTO HIROMASA ,  KAWAI KOJI ,  MIKI HISAYA

IPC: B41M5/145 ,  B41M5/30 ,  B41M5/327 ,  C07D493/22 ,  C09B11/28

Abstract: PURPOSE:To provide the subject compound useful as a color-developable dye in color-developable recording materials such as thermosensitive recording sheet and pressure-sensitive recording sheet. CONSTITUTION:The objective compound of formula I (R and R are each 1-9C alkyl or 3-6C cycloalkyl; R is H or anilino; R is H or 1-4C alkyl), for example, a compound of formula II. This compound is obtained by reaction of (A) a novel aromatic diketodicarboxylic acid of formula III with (B) a 4- alkoxydiphenylamine derivative of formula IV (R is lower alkyl). The novel compound of the formula III can be prepared by reaction of (1) a m-aminophenol derivative with (2) pyromellitic dianhydride.

公开(公告)号：JPH0418060A

公开(公告)日：1992-01-22

申请号：JP12178290

申请日：1990-05-11

Applicant: MITSUI PETROCHEMICAL IND

Inventor： TANAKA MICHIO ,  TARUMOTO HIROMASA ,  KAWAI KOJI ,  MIKI HISAYA

IPC: C07C227/10 ,  C07C229/52

Abstract: NEW MATERIAL:An aromatic diketodicarboxylic acid expressed by formula I (R and R are 1-9C alkyl or 3-6C cycloalkyl). EXAMPLE:2,5-Bis(4'-N,N-diethylamino)-(2'-hydroxybenzoyl)terephthalic acid. USE:Useful as a raw material for producing fluoran compounds used as a coloring dye for coloring recording materials such as heat-sensitive recording paper and pressure-sensitive paper. Since the new compound expressed by formula I especially has two sets of symmetric ketone groups and carboxyl groups in the molecule, the compound is effectively used as a raw material for producing the fluoran compounds having the two fluoran structures in the molecule. PREPARATION:An m-aminophenol derivative expressed by formula II is reacted with pyromellitic anhydride in a solvent such as toluene to afford the compound expressed by formula I at 30-160 deg.C, preferably 40-120 deg.C.

公开(公告)号：JPH0212209B2

公开(公告)日：1990-03-19

申请号：JP3726582

申请日：1982-03-11

Applicant: MITSUI PETROCHEMICAL IND

Inventor： NAKAGAWA HIROAKI ,  MIZUNO KENICHI ,  MATSUMOTO TETSUHIRO ,  TARUMOTO HIROMASA

IPC: C07C37/86 ,  C07C27/00 ,  C07C37/08 ,  C07C39/10 ,  C07C67/00 ,  C07C303/20 ,  C07C309/25

公开(公告)号：JPS58157737A

公开(公告)日：1983-09-19

申请号：JP3726582

申请日：1982-03-11

Applicant: MITSUI PETROCHEMICAL IND

Inventor： NAKAGAWA HIROAKI ,  MIZUNO KENICHI ,  MATSUMOTO TETSUHIRO ,  TARUMOTO HIROMASA

IPC: C07C37/86 ,  C07C27/00 ,  C07C37/08 ,  C07C39/10 ,  C07C67/00 ,  C07C303/20 ,  C07C309/25

Abstract: PURPOSE:Phlorogrucinol is selectively converted into a water-soluble compound with an alkali hydrogensulfite and separated from oil-soluble contaminants, then the product is subjected to elimination reaction to give readily high-quality phlorogrucinol from its crude product. CONSTITUTION:The oxidation product of 1,3,5-triisopropylbenzene mainly containing trihydroperoxide is decomposed in the presence of an acidic catalyst to give a crude phlorogrucinol. Then, the product is heated together with an alkali hydrogensulfite in the presence of water to give selectively water-soluble 1,3,5- trihydroxycyclohexane-1,3,5-trisulfonic acid trialkali salt. The reaction mixture is separated into the aqueous layer containing the above water-soluble compound and the oily layer containing contaminants. The aqueous layer is, preferably after purified, treated with an acid or base to effect elimination reaction to give high-quality phlorogrucinol.

公开(公告)号：JPS58150529A

公开(公告)日：1983-09-07

申请号：JP3177882

申请日：1982-03-02

Applicant: MITSUI PETROCHEMICAL IND

Inventor： NAKAGAWA HIROAKI ,  MIZUNO KENICHI ,  MATSUMOTO TETSUHIRO ,  TARUMOTO HIROMASA

IPC: C07C37/08 ,  B01J27/02 ,  C07B61/00 ,  C07C27/00 ,  C07C39/10 ,  C07C67/00

Abstract: PURPOSE:To prepare phloroglucin which is an intermediate for medicines or agricultural chemicals in high yield, by oxidizing 1,3,5-triisopropylbenzene, oxidizing further the resultant oxidation product mixture in the presence of hydrogen peroxide, and decomposing the resultant oxidation product. CONSTITUTION:(i) 1,3,5-Triisopropylbenzene is oxidized with O2 gas under heating to give a mixture of trihydroperoxide of 1,3,5-triisopropylbenzene with a monocarbinol dihydroperoxide, a dicarbinol monohydroperoxide and tricarbinol. The resultant mixture is then brought into contact with hydrogen peroxide in the presence of an acidic catalyst and oxidized to afford an oxidation product consisting essentially of the trihydroperoxide, which is then decomposed in the presence of an acidic catalyst to give an acidic decomposition reaction mixture. The aimed phloroglucin is separated from the resultant mixture.