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    METHOD FOR PRODUCING TERPYRIDINE
    3.
    发明专利
    METHOD FOR PRODUCING TERPYRIDINE 审中-公开

    公开(公告)号：JP2002363161A

    公开(公告)日：2002-12-18

    申请号：JP2002131389

    申请日：2002-05-07

    Applicant: BASF AG

    Inventor： LUNKWITZ RALPH ,  PABST GUNTHER ,  SCHERR GUENTER DR

    IPC: C07D401/14 ,  C07D213/50 ,  C07D213/61 ,  C07D213/68 ,  C07D213/803

    Abstract: PROBLEM TO BE SOLVED: To provide a method for producing terpyridine from 2-cyanopyridine on an industrial scale. SOLUTION: Terpyridine is produced by a method containing a successive reaction process comprising (A) the condensation of a (1-4C alkyl)pyridine-2- carboxylate derivative and acetone in an aprotic solvent in the presence of a base, (B) the reaction of the obtained 1,5-bis(2-pyridyl)pentane-1,3,5-trione derivative with ammonia or an ammonium salt of the formula: (NH4 )q Y while removing produced water from the system and (C) the chlorination of the obtained 2,6-bis(2-pyridyl)-4(1H)pyridinone derivative.

    PRODUCTION OF GUANIDINE DERIVATIVE
    4.
    发明专利
    PRODUCTION OF GUANIDINE DERIVATIVE 失效

    公开(公告)号：JP2000191625A

    公开(公告)日：2000-07-11

    申请号：JP36247499

    申请日：1999-12-21

    Applicant: BASF AG

    Inventor： KESSEL KNUT ,  KLUGE MICHAEL DR ,  GREINDL THOMAS DR ,  BOGENSTAETTER THOMAS DR ,  SCHERR GUENTER DR ,  RAULS MATTHIAS DR ,  VAN GELDER RICHARD

    IPC: C07C277/08 ,  C07C279/14 ,  C07C303/22 ,  C07C309/15 ,  C07F9/38

    Abstract: PROBLEM TO BE SOLVED: To readily obtain a guanidine derivative in a high purity, high yield and narrow particle size distribution by reacting O-alkyl isourea salt with a specific amine in the presence of a seed crystal of a guanidine derivative. SOLUTION: This guanidine derivative (A) is expressed by formula I [R1 is a 1-8C alkylene or a 5-10C bifunctional alicyclic group; R2 is H or a 1-8C alkyl; Z is COOR3, SO2R3 (R3 is H, an alkali metal or the like) or the like] and is obtained by reacting (B) an O-alkyl isourea salt of formula II (R5 is a 1-8C alkyl; X- is 1 equivalent of anion) with (C) an amine of formula III in the presence of (D) a seed crystal of a guanidine of formula I. Preferably, the reaction is performed in a reaction chamber in which the components B and C are continuously introduced and thereafter the crystal of the component D is continuously taken out.

    PRODUCTION OF SUBSTITUTED GUANIDINE DERIVATIVE
    6.
    发明专利
    PRODUCTION OF SUBSTITUTED GUANIDINE DERIVATIVE 失效

    公开(公告)号：JPH11209335A

    公开(公告)日：1999-08-03

    申请号：JP31219798

    申请日：1998-11-02

    Applicant: BASF AG

    Inventor： GREINDL THOMAS DR ,  SCHERR GUENTER DR ,  SCHNEIDER ROLF ,  MUNDINGER KLAUS DR

    IPC: C07C277/02 ,  C07C277/08 ,  C07C279/14 ,  C07C303/22 ,  C07C303/30 ,  C07C303/40 ,  C07C309/15 ,  C07C309/69 ,  C07C311/47

    Abstract: PROBLEM TO BE SOLVED: To obtain the subject high-purity compound simply in a high yield by using readily obtainable starting raw materials, by reacting calcium cyanamide with a primary or a secondary aminocarboxylic acid. SOLUTION: Calcium cyanamide is reacted with a primary or a secondary aminocarboxylic acid alcohol of the formula I [R is H or a 1-20C alkyl; R is a (1-20C alkylene)-COOR , a (1-20C alkylene)-CONR R (R is H, a 3-8C cycloalkyl or the like; R and R are each H, a 6-18C aryl or the like) or the like], a primary or a secondary aminosulfonic acid or their derivative to give the objective compound of formula II. Preferably the reaction is carried out in water and/or an organic solvent mixable with water at 40-80 deg.C at pH 9-11. Preferably calcium cyanamide is economically used in the form of industrial lime nitrogen containing 30-95 wt.% of calcium cyanamide. Sarcosine sodium or potassium salt is preferable as the compound of formula I or its derivative.

    PRODUCTION OF GUANIDINE DERIVATIVE
    7.
    发明专利
    PRODUCTION OF GUANIDINE DERIVATIVE 失效

    公开(公告)号：JP2000229936A

    公开(公告)日：2000-08-22

    申请号：JP2000031893

    申请日：2000-02-09

    Applicant: BASF AG

    Inventor： KESSEL KNUT ,  KLUGE MICHAEL DR ,  BOGENSTAETTER THOMAS DR ,  SCHERR GUENTER DR

    IPC: C07C277/02 ,  C07C277/08 ,  C07C279/14

    Abstract: PROBLEM TO BE SOLVED: To easily and continuously produce a guanidine derivative in a high purity and in a high yield by continuously reacting a cyanamide derivative with an amine in the presence of the seed crystals of the guanidine derivative. SOLUTION: This method for producing a guanamide derivative of formula III (R5, R6 are each H or a 1-8C alkyl) comprises continuously reacting a cyanamide derivative of formula I [R5', R6' are each H, the equivalent of an alkali(ne earth) metal or a 1-8C alkyl] with an amine of formula II R1 is a 1-8C alkylene or a 5-10C divalent alicyclic group; R2 is H or a 1-8C alkyl, or R1 and R2 form a Z-substituted five or six-membered ring together with the N atom bound to R1 and R2; and Z is COOR3 [R3 is H or the equivalent of an alkali(ne earth) metal] or the like) (for example, an amino carboxylic acid, an amino sulfonic acid or an amino phosphoric acid) in the presence of the seed crystals of the formula III. The cyanamide derivative of formula I and the amine of formula II are preferably used in a molar ratio of 2:1 to 1:2, and the reaction is carried out at pH 8-12 in an aqueous medium.

    PRODUCTION OF O-ALKYL ISOUREA
    8.
    发明专利
    PRODUCTION OF O-ALKYL ISOUREA 失效

    公开(公告)号：JP2000159742A

    公开(公告)日：2000-06-13

    申请号：JP33181799

    申请日：1999-11-22

    Applicant: BASF AG

    Inventor： KLUGE MICHAEL DR ,  KESSEL KNUT ,  GREINDL THOMAS DR ,  BIEDERMANN NORBERT DR ,  SCHERR GUENTER DR ,  BOGENSTAETTER THOMAS DR

    IPC: C07C273/18 ,  C07C273/00 ,  C07C275/70

    Abstract: PROBLEM TO BE SOLVED: To obtain an O-alkyl isourea as an acid adduct salt in a high yield, if necessary, by dissolving and dispersing urea and an alkyl group donor in a diluent, followed by reacting them in a continuously operated reactor at a specific temperature. SOLUTION: An O-alkyl isourea shown by the formula (R1 is a 1-20C alkyl) is obtained as an acid adduct salt in a high yield, if necessary, by dissolving and dispersing (a) urea and (B) an alkyl group donor (e.g. dialkyl sulfate) in a diluent, followed by reacting them in a continuously operated reactor (e.g. continuously flowed column reactor and continuously stirred tank reactor) at 40-200 deg.C. It is preferable that an (A:B) molar ratio is (3:1)-(1:2). The diluent has a heat capacity which elevates the temperature of the reaction mixture maximally to 150 deg.oC or less upon performing a substantially adiabatic reaction by the heat of the reaction.

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