PURIFICATION AND PRODUCTION OF 2,3,5-TRIMETHYL- PARABENZOQUINONE BY CATALYTIC OXIDATION

    公开(公告)号:JP2000143576A

    公开(公告)日:2000-05-23

    申请号:JP28592699

    申请日:1999-10-06

    Applicant: BASF AG

    Abstract: PROBLEM TO BE SOLVED: To provide a method for purifying or isolating 2,3,5-trimethyl-p- benzoquinone by surely removing intermediates and by-products formed during production of the compound and avoiding degradation of the component by diminishing the thermal stress caused by the treatment by separating the compound by the crystallization. SOLUTION: A method is provided for purifying 2,3,5-trimethyl-p-benzoquinone (TMQ) or isolating TMQ from a TMQ-containing mixture by separating by crystallizing preferably at -6 to 32 deg.C. A TMQ-containing mixture to be purified or TMQ contains TMQ preferably at 1-99.999 wt.%, more preferably at 90-99.999 wt.%. The TMQ-containing mixture is formed preferably by the catalytic oxidation of trimethylphenol. TMQ is a useful intermediate for the production of trimethylhydroquinone which is a precursor for the synthesis of α-tocopherol.

    PRODUCTION OF CHROMANOL DERIVATIVE

    公开(公告)号:JP2000095776A

    公开(公告)日:2000-04-04

    申请号:JP26767299

    申请日:1999-09-21

    Applicant: BASF AG

    Abstract: PROBLEM TO BE SOLVED: To economically and safely obtain the subject compound useful as a biological agent by reaction of a specific oxochromanol derivative with metallic zinc in the presence of an acid or the like to effect reduction of the derivative so as not to change the double bond form or the like in the unsaturated side chain by isomerization or the like. SOLUTION: This compound of formula II (e.g. γ-tocotrienol) is obtained by reaction of a 4-oxo-chromanol derivative of formula I ((n) is 1-10; R1 to R4 are each H or a 1-4C alkyl; R5 is H, a 1-4C alkyl or the like) (e.g. 4-oxo-γ- tocotrienol) with a metallic zinc pref. at 1-0 molar equivalent based on the compound of formula I in the presence of an acid or acid mixture (pref. hydrochloric acid) pref. in an organic solvent such as n-heptane pref. at 20-100 deg.C normally 10 min to 24 h to effect reduction of the derivative of formula I.

    PRODUCTION OF 2,5,6-TRIMETHYL-2-CYCLOHEXEN-1-ONE

    公开(公告)号:JPH11292819A

    公开(公告)日:1999-10-26

    申请号:JP6492199

    申请日:1999-03-11

    Applicant: BASF AG

    Abstract: PROBLEM TO BE SOLVED: To provide a method for producing 2,5,6-trimethyl-2-cyclohexen-1-one in industrial scale, good yield and good space time yield. SOLUTION: This method for producing 2,5,6-trimethyl-2-cyclohexen-1-on comprises simultaneously pumping 1 mol crotonaldehyde or 1 mol compound which is converted under the reaction conditions into crotonaldehyde, about 5-30 mol diethyl ketone and the aqueous solution or suspension of a strong base in the presence of a base agent at elevated temperature, through separate lines or at least partly in the form of a suitable mixture, continuously into a pressure vessel, which is heated where appropriate and which ensures vigorous mixing, in such a way that the reaction temperature is 150-350 deg.C and the average residence time in the pressure vessel is about 0.1 second to 20 min.

    4.
    发明专利
    未知

    公开(公告)号:DK1094056T3

    公开(公告)日:2004-03-29

    申请号:DK00120644

    申请日:2000-09-21

    Applicant: BASF AG

    Abstract: Preparation of monoacetylated hydroquinone compound comprises reacting a dicetylphenol compound with peroxo compounds optionally using an acid in one reaction step. Preparation of monoacetylated hydroquinone compound of formula (I) comprises reacting a dicetylphenol compound of formula (II) with peroxo compounds optionally using an acid. R1-R3 = H or Me. Independent claims are included for: (1) preparation of (II) by reacting phenol compounds of formula (III) with an acetylation agent using an acid catalyst; (2) preparation of monoacetylated hydroquinone compounds (I) by reacting (III) with an acetylation agent using an acid catalyst to give (II) and further reacting with peroxo compounds, optionally in the presence of an acid; and (3) compounds of formula (Ia)-(Ie).

    5.
    发明专利
    未知

    公开(公告)号:ES2215533T3

    公开(公告)日:2004-10-16

    申请号:ES00120644

    申请日:2000-09-21

    Applicant: BASF AG

    Abstract: Preparation of monoacetylated hydroquinone compound comprises reacting a dicetylphenol compound with peroxo compounds optionally using an acid in one reaction step. Preparation of monoacetylated hydroquinone compound of formula (I) comprises reacting a dicetylphenol compound of formula (II) with peroxo compounds optionally using an acid. R1-R3 = H or Me. Independent claims are included for: (1) preparation of (II) by reacting phenol compounds of formula (III) with an acetylation agent using an acid catalyst; (2) preparation of monoacetylated hydroquinone compounds (I) by reacting (III) with an acetylation agent using an acid catalyst to give (II) and further reacting with peroxo compounds, optionally in the presence of an acid; and (3) compounds of formula (Ia)-(Ie).

    6.
    发明专利
    未知

    公开(公告)号:DE19649564A1

    公开(公告)日:1998-06-04

    申请号:DE19649564

    申请日:1996-11-29

    Applicant: BASF AG

    Abstract: Improved method for the production of gamma , delta -unsaturated ketones desired as odoriferous substances or as intermediate products for vitamins or carotinoids by the reaction of tertiary allyl alcohols and alkenyl alkyl ethers in the presence of acid catalyzers at high temperature. It is characterized in that the reaction is carried out in the presence of a phosphorus derivative of general formula (IV), in which A and B stand for a branched or unbranched alkyl or alkoxy radical with 1 to 10 C atoms, an optionally substituted aryl radical, cycloalkyl radical, aryloxy radical or cycloalkyloxy radical. In addition, A can stand for -H or -OH, or A and B together stand for an optionally substituted tetramethylene or pentamethylene radical, or for an optionally substituted phenyl-1,2-diol radical or a 1,1'-binaphthyl-2,2'-diol radical.

    7.
    发明专利
    未知

    公开(公告)号:AT260236T

    公开(公告)日:2004-03-15

    申请号:AT00120644

    申请日:2000-09-21

    Applicant: BASF AG

    Abstract: Preparation of monoacetylated hydroquinone compound comprises reacting a dicetylphenol compound with peroxo compounds optionally using an acid in one reaction step. Preparation of monoacetylated hydroquinone compound of formula (I) comprises reacting a dicetylphenol compound of formula (II) with peroxo compounds optionally using an acid. R1-R3 = H or Me. Independent claims are included for: (1) preparation of (II) by reacting phenol compounds of formula (III) with an acetylation agent using an acid catalyst; (2) preparation of monoacetylated hydroquinone compounds (I) by reacting (III) with an acetylation agent using an acid catalyst to give (II) and further reacting with peroxo compounds, optionally in the presence of an acid; and (3) compounds of formula (Ia)-(Ie).

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