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    PRODUCTION OF GUANIDINE DERIVATIVE
    1.
    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 GUANIDINE DERIVATIVE
    2.
    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
    3.
    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.

    METHOD FOR PURIFYING CREATINE
    5.
    发明专利
    METHOD FOR PURIFYING CREATINE 失效

    公开(公告)号：JP2001181254A

    公开(公告)日：2001-07-03

    申请号：JP2000387369

    申请日：2000-12-20

    Applicant: BASF AG

    Inventor： KESSEL KNUT ,  SCHERR GUENTER DR ,  BOGENSTAETTER THOMAS DR ,  ORSTEN STEFAN ,  FRANKE DIRK

    IPC: C07C277/06 ,  C07C277/08 ,  C07C279/14

    Abstract: PROBLEM TO BE SOLVED: To provide a method for providing creatine having purity as high as possible in a simple way. SOLUTION: A method for purifying creatine is to introduce creatine to be purified and not containing water of crystallization into a saturated aqueous solution of creatine monohydrate in such a way that the creatine not containing water of crystallization is dissolved under a hydrated condition, to precipitate the crystal of creatine monohydrate from the aqueous solution and to separate the above crystal from the aqueous solution.

    8.
    发明专利
    未知

    公开(公告)号：DE50001372D1

    公开(公告)日：2003-04-10

    申请号：DE50001372

    申请日：2000-12-21

    Applicant: BASF AG

    Inventor： KESSEL KNUT ,  SCHERR GUENTER ,  BOGENSTAETTER THOMAS ,  ORSTEN STEFAN ,  FRANKE DIRK

    IPC: C07C277/06 ,  C07C277/08 ,  C07C279/14

    Abstract: Purification of creatine (I) involves adding the (I) to be purified, in anhydrous form, to a saturated aqueous solution of (I) monohydrate, so that the anhydrous (I) is dissolved with hydration, then separating the crystals of (I) monohydrate which precipitate from the solution. An Independent claim is also included for the preparation of (I) monohydrate, by: (a) reacting sarcosine with an guanylating agent in an aqueous medium, so that crude (I) monohydrate is precipitated; (b) separating the crude product form the medium; (c) optionally washing; (d) converting the product into anhydrous (I); (e) adding the anhydrous (I) to a saturated aqueous solution of (I) monohydrate, so that the anhydrous (I) is dissolved with hydration; (f) separating the crystals of (I) monohydrate which precipitate from the solution; and (g) utilizing the aqueous solution at least partially as aqueous medium in step (a) and/or washing liquid in step (c).

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