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    PRODUCTION OF O-ALKYL ISOUREA
    2.
    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.

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

    公开(公告)号：JPH11209334A

    公开(公告)日：1999-08-03

    申请号：JP31219598

    申请日：1998-11-02

    Applicant: BASF AG

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

    IPC: C07C277/02 ,  C07C273/18 ,  C07C275/70 ,  C07C277/08 ,  C07C279/04 ,  C07C279/14 ,  C07C303/22 ,  C07C303/30 ,  C07C309/15 ,  C07C309/69 ,  C07C311/47 ,  C08G65/333 ,  C08G73/02

    Abstract: PROBLEM TO BE SOLVED: To obtain the subject high-purity compound simply, economically in a high yield from readily obtainable starting substances, by reacting calcium cyanamide with an alcohol and reacting the obtained isourea derivative with a primary or a secondary amine. SOLUTION: Calcium cyanamide is reacted with an alcohol of the formula, R -OH (R is a 1-20C alkyl) preferably in the presence of an inorganic acid at 0-25 deg.C to give an isourea derivative of formula I. Then, the compound of formula I is reacted with a primary or a secondary amine of formula II (R is H, a 1-20C alkyl or the like; R is a 1-20C alkyl, a 2-20C alkenyl or the like) preferably at 20-40 deg.C at pH 9-10 to give the objective compound of formula III. 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 II.

    PRODUCTION OF GUANIDINE DERIVATIVE
    6.
    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
    8.
    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.

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