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    4.
    发明专利
    未知

    公开(公告)号：MX173525B

    公开(公告)日：1994-03-14

    申请号：MX363586

    申请日：1986-09-03

    Applicant: HOECHST AG

    Inventor： SCHWEIKERT OTTO ERNST ,  MACK KARL ERNST ,  REUSCHLING DIETER ,  LINKIES ADOLF ,  REIMANN WALTER

    IPC: A23L27/20 ,  A23L27/30 ,  C07D291/06

    Abstract: 6-Methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide is prepared by cylcizing acetoacetamide-N-sulfonic acid or its salts with an at least approximately equimolar amount of SO3 in the presence of a water-immiscible, inert organic solvent and, if appropriate, also an inert, inorganic solvent. In the event that an equimolar amount of SO3 is employed, working up is effected by adding aqueous sulfuric acid when the cyclization reaction is complete; in the event that the amount of SO3 employed is more than equimolar, the 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide obtained in the form of the SO3-adduct is hydrolyzed by adding water or ice, whereby sulfuric acid is formed from the SO3 combined in the SO3-adduct. The inert, organic solvent is then removed from the resulting multi-phase mixture by distillation, and the 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide is obtained in a pure form from the remaining aqueous sulfuric acid phase by crystallization. Additionally, quite generally, crude 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide is purified by recrystallization from aqueous sulfuric acid. The non-toxic salts of 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2 dioxide-in particular the potassium salt-are valuable synthetic sweetening agents.

    5.
    发明专利
    未知

    公开(公告)号：DK168286B1

    公开(公告)日：1994-03-07

    申请号：DK126185

    申请日：1985-03-20

    Applicant: HOECHST AG

    Inventor： LINKIES ADOLF ,  REUSCHLING DIETER

    IPC: B01J27/00 ,  B01J27/232 ,  A23L27/30 ,  C07B61/00 ,  C07C67/00 ,  C07C301/00 ,  C07C303/36 ,  C07C307/00 ,  C07C307/02 ,  C07C311/00 ,  C07D291/06

    Abstract: Crystalline salts of acetoacetamide-N-sulfofluoride are prepared by reacting amidosulfofluoride H2NSO2F with diketene in the presence of inorganic bases, preferably alkali metal carbonates and/or hydrogencarbonates, in particular potassium carbonate, in an inert organic solvent. The salts can be further processed with further base, for example with methanolic KOH, into salts of 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one-2,2-dioxide; the potassium salt, in particular, is important for use as a sweetener ("Acesulfame").

    6.
    发明专利
    未知

    公开(公告)号：DK168043B1

    公开(公告)日：1994-01-24

    申请号：DK129285

    申请日：1985-03-21

    Applicant: HOECHST AG

    Inventor： CLAUSS KARL ,  LINKIES ADOLF ,  REUSCHLING DIETER

    IPC: A23L27/30 ,  C07D291/06

    Abstract: 6-Methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide is prepared by reaction of acetoacetamide with at least approximately twice the molar amount of SO3 per mole of acetoacetamide, if appropriate in an inert inorganic or organic solvent. Relevant salts can be obtained, using bases, from the product which results in the form of the acid. The non-toxic salts, in particular the potassium salt, are valuable synthetic sweeteners.

    7.
    发明专利
    未知

    公开(公告)号：NO166364C

    公开(公告)日：1991-07-10

    申请号：NO854604

    申请日：1985-11-18

    Applicant: HOECHST AG

    Inventor： CLAUSS KARL ,  LINKIES ADOLF ,  REUSCHLING DIETER

    IPC: A23L27/30 ,  B01J31/00 ,  B01J31/02 ,  B01J31/24 ,  C07B61/00 ,  C07C303/34 ,  C07C307/02 ,  C07C311/46 ,  C07D291/06

    Abstract: 6-Methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide is prepared by (a) reacting, in an inert organic solvent, a salt of sulfamic acid, which is at least partially soluble therein, with at least approximately the equimolar amount of an acetoacetylating agent, in the presence of an amine or phosphine catalyst, and by cyclizing the acetoacetamide-N-sulfonate which is formed in this reaction, or the free sulfonic acid, (b) by the action of at least approximately the equimolar amount of SO3, where appropriate in an inert inorganic or organic solvent, to give 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide, which is produced in the form of the acid in this reaction; it is possible, if desired, to obtain from the acid form (c) the appropriate salts by neutralization with bases. The non-toxic salts - in particular the potassium salt - are valuable synthetic sweeteners.

    8.
    发明专利
    未知

    公开(公告)号：MX162880B

    公开(公告)日：1991-07-02

    申请号：MX20470385

    申请日：1985-03-22

    Applicant: HOECHST AG

    Inventor： CLAUSS KARL ,  LINKIES ADOLF ,  REUSCHLING DIETER

    IPC: A23L27/30 ,  B01J31/00 ,  B01J31/02 ,  B01J31/24 ,  C07B61/00 ,  C07C303/34 ,  C07C307/02 ,  C07C311/46 ,  C07D291/06

    Abstract: 6-Methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide is prepared by (a) reacting, in an inert organic solvent, a salt of sulfamic acid, which is at least partially soluble therein, with at least approximately the equimolar amount of an acetoacetylating agent, in the presence of an amine or phosphine catalyst, and by cyclizing the acetoacetamide-N-sulfonate which is formed in this reaction, or the free sulfonic acid, (b) by the action of at least approximately the equimolar amount of SO3, where appropriate in an inert inorganic or organic solvent, to give 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide, which is produced in the form of the acid in this reaction; it is possible, if desired, to obtain from the acid form (c) the appropriate salts by neutralization with bases. The non-toxic salts - in particular the potassium salt - are valuable synthetic sweeteners.

    PROCESS FOR THE PREPARATION OF 6-METHYL-3,4-DIHYDRO-1, 2,3-OXATHIAZIN-4-ONE 2,2-DIOXIDE AND FOR THE PURIFICATION THEREOF
    10.
    发明专利
    PROCESS FOR THE PREPARATION OF 6-METHYL-3,4-DIHYDRO-1, 2,3-OXATHIAZIN-4-ONE 2,2-DIOXIDE AND FOR THE PURIFICATION THEREOF 未知

    公开(公告)号：CA1283912C

    公开(公告)日：1991-05-07

    申请号：CA517244

    申请日：1986-08-29

    Applicant: HOECHST AG

    Inventor： REUSCHLING DIETER ,  LINKIES ADOLF ,  REIMANN WALTER ,  SCHWEIKERT OTTO E ,  MACK KARL E

    IPC: A23L27/20 ,  A23L27/30 ,  C07D291/06

    Abstract: of the disclosure: 6-Methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide is prepared by cyclizing acetoacetamide-N-sulfonic acid or its salts with an at least approximately equimolar amount of SO3 in the presence of a water-immiscible, inert organic solvent and, if appropriate, also an inert, inorganic solvent. In the event that an equimolar amount of SO3 is employed, working up is effected by adding aqueous sulfuric acid when the cyclization reaction is complete; in the event that the amount of SO3 employed is more than equimolar the 6-methyl-3,4-dihydro-1,2,3-oxa-thiazin-4-one 2,2-dioxide obtained in the form of the SO3-adduct is hydrolyzed by adding water or ice, whereby sulfuric acid is formed from the SO3 combined in the SO3adduct. The inert, organic solvent is then removed from the resulting multi-phase mixture by distillation, and the 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide is obtained in a pure form from the remaining aqueous sulfuric acid phase by crystallization. Additionally, quite generally, crude 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide is purified by recrystallization from aqueous sulfuric acid. The non-toxic salts of 6-methyl-3,4-dihydro-1,2,3-oxa-thiazin-4-one 2,2-dioxide - in particular the potassium salt - are valuable synthetic sweetening agents.

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