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    PRODUCTION OF CRYSTALLINE SOLID FROM GLYCINE-N,N-DIACETIC DERIVATIVE HAVING SUFFICIENTLY LOW HYGROSCOPIC PROPERTY
    1.
    发明专利
    PRODUCTION OF CRYSTALLINE SOLID FROM GLYCINE-N,N-DIACETIC DERIVATIVE HAVING SUFFICIENTLY LOW HYGROSCOPIC PROPERTY 失效

    公开(公告)号：JPH10175929A

    公开(公告)日：1998-06-30

    申请号：JP32491397

    申请日：1997-11-26

    Applicant: BASF AG

    Inventor： SCHOENHERR MICHAEL DR ,  RAULS MATTHIAS DR ,  ASCHERL HERMANN ,  LETZELTER THOMAS ,  BAUMANN DIETER ,  POTTHOFF-KARL BIRGIT DR

    IPC: C11D1/04 ,  C07C227/42 ,  C07C229/16 ,  C07C229/24

    Abstract: PROBLEM TO BE SOLVED: To obtain a crystalline solid of the subject compound substantially not containing an additive and having virtually sufficiently low hygroscopic property. SOLUTION: This crystalline solid constituted of a glycine-N,N-diacetic acid derivative represented by formula I [R is a 1-30C alkyl or a 2-30C alkenyl, a group of formula II (A is a 1-12C alkylene bridge, etc.; M is H or an alkali metal, etc.), etc.] is produced by distilling away water content of an aqueous solution of (A) glycine-N,N-diacetic acid derivative I [R is a 1-20C alkyl or a group of formula II, etc.] as a starting substance. Crystallization is carried out by adding a crystalline component A in an amount of 0.001-50wt.%, preferably 0.01-10wt.% based on an amount of the component A in a starting substance as a nucleus for crystallization and the crystallization temperature is controlled to 10-100 deg.C, especially 40-80 deg.C. The resultant crystalline solid has a purity of 70-99.9%, especially 80-99.5% based on total amount of solid.

    6.
    发明专利
    未知

    公开(公告)号：AT202075T

    公开(公告)日：2001-06-15

    申请号：AT97119147

    申请日：1997-11-03

    Applicant: BASF AG

    Inventor： SCHOENHERR MICHAEL DR ,  RAULS MATTHIAS DR ,  ASCHERL HERMANN ,  LETZELTER THOMAS ,  BAUMANN DIETER ,  POTTHOFF-KARL BIRGIT DR

    IPC: C11D1/04 ,  C07C227/42 ,  C07C229/16 ,  C07C229/24

    Abstract: A method for the preparation of a crystalline solid comprising a glycine-N,N-diacetic acid derivative of formula (I) with a very low hygroscopicity, comprises fixing the water content of the starting material containing (I) at 10-30 wt.% and then carrying out crystallisation: MOOC-CH(R)-N(CH2COOM)2 (I) R = 1-30C alkyl or 2-30C alkenyl (both optionally containing 1-5 OH, formyl, 1-4C alkoxy(carbonyl) or phenoxy groups and/or optionally containing up to 5 non-adjacent O atoms in the chain), alkoxylate groups of formula (II), phenyl-(1-20 C)-alkyl (optionally containing up to 3 1-4C alkyl, OH, carboxyl, sulpho or 1-4C alkoxycarbonyl ring substituents), 5- or 6-membered optionally benzalated heterocyclic ring containing up to 3 N, O or S atoms (optionally containing up to 3 1-4C alkyl, OH, carboxyl, sulpho or 1-4C alkoxycarbonyl substituents) or a group of formula (III): -(CH2)k-O-(A O)m-(A O)n-Y (II) -A-CH(COOM)-N(CH2COOM)2 (III) A , A = 2-4C 1,2-alkylene; Y = H, 1-12C alkyl, phenyl or 1-4C alkoxycarbonyl; k = 1-3; m, n = 0-50; A = 1-12C alkylene or single bond; and M = H, alkali(ne earth) metal or optionally substituted ammonium, with the provision that m+n = at least 4.

    Prodn. of 3,4-di:hydro-isoquinoline or deriv.
    7.
    发明专利
    Prodn. of 3,4-di:hydro-isoquinoline or deriv. 未知

    公开(公告)号：DE19507522A1

    公开(公告)日：1996-09-05

    申请号：DE19507522

    申请日：1995-03-03

    Applicant: BASF AG

    Inventor： WEHLAGE THOMAS DR ,  KAPPES ELISABETH DR ,  OFTRING ALFRED DR ,  SCHOENHERR MICHAEL DR ,  BECKER RAINER DR

    IPC: C07D217/02 ,  C07D217/04

    Abstract: Prodn. of 3,4-dihydro-isoquinoline cpds. of formula (I) comprises oxidising 1,2,3,4-tetrahydro-isoquinoline cpds. of formula (II) with NaOCl and/or KOCl in the absence of organic solvents. R2, R3 = R' or R"; R' = 1-20C alkyl, up to 20C cycloalkyl or aryl (all opt. substd. by aryl, NO2, CN, halogen, 1-20C alkyl, amino, 1-20 aminoalkyl, 1-20C thioalkyl, 1-20 sulphoalkyl, carboxylate ester, OH, 1-20C alkoxy, polyalkoxy or 1-40C quaternised di- or tri- alkylammonium or carboxyalkyl), H or heterocyclyl; R" = NO2, halo, CN, 1-20C alkoxy, phenoxy, benzyloxy, keto, COOH, 1-20C carboalkoxy, NH2 or mono- or di(1-6C alkyl)amino. Also claimed is a process as above where the prod. is quaternised with R1X to give a 3,4-dihydro-isoquinolinium salt of formula (III). R1 = R'; X = oxidn.-stable anion, pref. Cl, Br, sulphate, methylsulphate, sulphonate, p-toluenesulphonate, boron tetrafluoride, phosphorus pentafluoride, phosphate, cyanide or ethylsulphate.

    9.
    发明专利
    未知

    公开(公告)号：DE19649681A1

    公开(公告)日：1998-06-04

    申请号：DE19649681

    申请日：1996-11-29

    Applicant: BASF AG

    Inventor： SCHOENHERR MICHAEL DR ,  RAULS MATTHIAS DR ,  ASCHERL HERMANN ,  LETZELTER THOMAS ,  BAUMANN DIETER ,  POTTHOFF-KARL BIRGIT DR

    IPC: C11D1/04 ,  C07C227/42 ,  C07C229/16 ,  C07C229/24 ,  C07C229/22 ,  C11D3/33

    Abstract: A method for the preparation of a crystalline solid comprising a glycine-N,N-diacetic acid derivative of formula (I) with a very low hygroscopicity, comprises fixing the water content of the starting material containing (I) at 10-30 wt.% and then carrying out crystallisation: MOOC-CH(R)-N(CH2COOM)2 (I) R = 1-30C alkyl or 2-30C alkenyl (both optionally containing 1-5 OH, formyl, 1-4C alkoxy(carbonyl) or phenoxy groups and/or optionally containing up to 5 non-adjacent O atoms in the chain), alkoxylate groups of formula (II), phenyl-(1-20 C)-alkyl (optionally containing up to 3 1-4C alkyl, OH, carboxyl, sulpho or 1-4C alkoxycarbonyl ring substituents), 5- or 6-membered optionally benzalated heterocyclic ring containing up to 3 N, O or S atoms (optionally containing up to 3 1-4C alkyl, OH, carboxyl, sulpho or 1-4C alkoxycarbonyl substituents) or a group of formula (III): -(CH2)k-O-(A O)m-(A O)n-Y (II) -A-CH(COOM)-N(CH2COOM)2 (III) A , A = 2-4C 1,2-alkylene; Y = H, 1-12C alkyl, phenyl or 1-4C alkoxycarbonyl; k = 1-3; m, n = 0-50; A = 1-12C alkylene or single bond; and M = H, alkali(ne earth) metal or optionally substituted ammonium, with the provision that m+n = at least 4.

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