公开(公告)号：WO2004043880A3

公开(公告)日：2004-07-29

申请号：PCT/EP0312458

申请日：2003-11-07

Applicant: BASF AG ,  DOMSCHKE THOMAS ,  MERGER MARTIN ,  GROSSMANN GEORG ,  FAUST TILLMANN

Inventor： DOMSCHKE THOMAS ,  MERGER MARTIN ,  GROSSMANN GEORG ,  FAUST TILLMANN

IPC: C07C20060101 ,  C07H7/027

CPC classification number: C07H7/027 ,  Y02P20/127

Abstract: The invention relates to a method for producing 2-keto-L-gulonic acid-C4-C10 alkyl ester by esterifying 2-keto-L-gulonic acid (KGS) with an unsaturated, branched or unbranched C4-C10 alcohol. The inventive method is characterized by the fact that an aqueous KGS solution is reacted with a C4-C10 alcohol up to an esterification degree of 20 to 70 percent in a pre-esterification process carried out under acidic catalysis conditions; and the obtained product is dehydrogenated with an unsaturated, branched or unbranched C4-C10 alcohol in a continuous rectification device, whereby the esterification reaction continues, n-butanol preferably being used as the alkyl alcohol. In a preferred embodiment, the aqueous KGS solution is concentrated up to or beyond the limit of solubility prior to the esterification process, preferably by catalyzing a homogeneous or heterogeneous catalyst, especially sulfonic acid, at temperatures of 50 to 120 °C. In another embodiment, the produced KGS ester is reacted in one or several additional steps so as to obtain L-ascorbic acid.

Abstract translation: 本发明涉及一种用于通过酯化2-酮基-L-古洛糖酸（KGA）与不饱和，支链或无支链的C 4 -C 10醇，其特征在于，生产2-酮基-L-古洛糖的C 4 -C 10烷基酯 即在初步反应酯化，水性KGA溶液用在酸催化下高达一定程度的20％至70％的酯化的C4-C10醇; 并且该产品是在与不饱和的，支链或无支链C4-C10醇的连续精馏装置脱水的进行，由此进行酯化反应。 优选地，烷基醇是正丁醇。 在一个优选的实施方案中，水性溶液KGA高达溶解度或超出之前酯化浓缩，优选在均相或非均相催化剂的催化，特别是硫酸，并在温度为50℃至120℃。 在所产生的KGS-酯为L-抗坏血酸的另一实施例中的一个或几个另外的步骤进行反应。

公开(公告)号：DE10231890B4

公开(公告)日：2004-07-01

申请号：DE10231890

申请日：2002-07-12

Applicant: BASF AG

Inventor： KAIBEL GERD ,  MERGER MARTIN ,  DOMSCHKE THOMAS ,  DECKERT PETRA ,  SAUER FRIEDRICH

IPC: C07D307/62 ,  C07C59/215

Abstract: The invention relates to a method for the separation of ascorbic acid from a mixture containing ascorbic acid and 2-keto-L-gulonic acid in a polar, preferably aqueous solvent, by means of liquid/liquid extraction using an amide. The method preferably also comprises steps for the back-extraction of the ascorbic acid, recycling of the extraction solvent and/or the back extraction solvent and for isolation of the ascorbic acid from the back extraction solvent. The invention further relates to a method for the production of ascorbic acid from KGA and isolation of the ascorbic acid so produced.

公开(公告)号：AU2003293666A1

公开(公告)日：2004-06-03

申请号：AU2003293666

申请日：2003-11-07

Applicant: BASF AG

Inventor： FAUST TILLMANN ,  DOMSCHKE THOMAS ,  MERGER MARTIN ,  GROSSMANN GEORG

IPC: C07C20060101 ,  C07H7/027

公开(公告)号：ES2124000T3

公开(公告)日：1999-01-16

申请号：ES95924972

申请日：1995-07-05

Applicant: BASF AG

Inventor： BOTT KASPAR ,  DOMSCHKE THOMAS ,  BOHN MICHAEL

IPC: B01J19/18 ,  C07C231/08 ,  C07C233/20

公开(公告)号：BRPI0405871A

公开(公告)日：2006-09-05

申请号：BRPI0405871

申请日：2004-12-28

Applicant: BASF AG

Inventor： KAIBEL GERD ,  MERGER MARTIN ,  DOMSCHKE THOMAS ,  DECKERT PETRA ,  SAUER FRIEDRICH

IPC: C07D307/62

公开(公告)号：CA2510026A1

公开(公告)日：2004-07-08

申请号：CA2510026

申请日：2003-12-13

Applicant: BASF AG

Inventor： DOMSCHKE THOMAS ,  MERGER MARTIN ,  SAUER FRIEDRICH ,  DECKERT PETRA

IPC: C07H1/06 ,  C07H7/027

Abstract: The invention relates to a method for extracting 2-ketone-L-gulonic acids fr om a polar, preferably aqueous solvent, preferably from a solvent which contain s a mixture of ascorbic acid and 2-ketone-L-gulonic acid, by means of liquid- liquid extraction with the aid of an extraction agent which contains a tertiary amine and a polar organic diluent. Preferably, the inventive method also comprises steps for retro-extracting the 2-ketone-L-gulonic acid and fo r returning the extraction agent. The invention also relates to a method for producing ascorbic acid from 2-ketone-L-gulonic acid and for isolating the thus produced ascorbic acid.

公开(公告)号：DE10231890A1

公开(公告)日：2004-02-05

申请号：DE10231890

申请日：2002-07-12

Applicant: BASF AG

Inventor： KAIBEL GERD ,  MERGER MARTIN ,  DOMSCHKE THOMAS ,  DECKERT PETRA ,  SAUER FRIEDRICH

IPC: C07D307/62

Abstract: The invention relates to a method for the separation of ascorbic acid from a mixture containing ascorbic acid and 2-keto-L-gulonic acid in a polar, preferably aqueous solvent, by means of liquid/liquid extraction using an amide. The method preferably also comprises steps for the back-extraction of the ascorbic acid, recycling of the extraction solvent and/or the back extraction solvent and for isolation of the ascorbic acid from the back extraction solvent. The invention further relates to a method for the production of ascorbic acid from KGA and isolation of the ascorbic acid so produced.

公开(公告)号：ES2250914T3

公开(公告)日：2006-04-16

申请号：ES03763731

申请日：2003-07-07

Applicant: BASF AG

Inventor： KAIBEL GERD ,  MERGER MARTIN ,  DOMSCHKE THOMAS ,  DECKERT PETRA ,  SAUER FRIEDRICH

IPC: C07D307/62

Abstract: Procedimiento para la separación de ácido ascórbico a partir de un disolvente 1 polar, que contiene ácido ascórbico y ácido 2-ceto-L-gulónico, caracterizado porque el procedimiento comprende el siguiente paso: (a) extracción de ácido ascórbico a partir del disolvente 1 con dialquilformamida (agente de extracción 1), que presenta un hueco de mezcla con el disolvente 1, en una extracción líquido-líquido.

公开(公告)号：DK1523477T3

公开(公告)日：2006-01-16

申请号：DK03763731

申请日：2003-07-07

Applicant: BASF AG

Inventor： KAIBEL GERD ,  MERGER MARTIN ,  DOMSCHKE THOMAS ,  DECKERT PETRA ,  SAUER FRIEDRICH

IPC: C07D307/62

Abstract: The invention relates to a method for the separation of ascorbic acid from a mixture containing ascorbic acid and 2-keto-L-gulonic acid in a polar, preferably aqueous solvent, by means of liquid/liquid extraction using an amide. The method preferably also comprises steps for the back-extraction of the ascorbic acid, recycling of the extraction solvent and/or the back extraction solvent and for isolation of the ascorbic acid from the back extraction solvent. The invention further relates to a method for the production of ascorbic acid from KGA and isolation of the ascorbic acid so produced.

公开(公告)号：DE10260085A1

公开(公告)日：2004-07-01

申请号：DE10260085

申请日：2002-12-19

Applicant: BASF AG

Inventor： DOMSCHKE THOMAS ,  MERGER MARTIN ,  DECKERT PETRA ,  SAUER FRIEDRICH

IPC: C07D307/62 ,  C07H7/027 ,  C07C59/215 ,  B01D11/04

Abstract: 2-Keto-L-gulonic acid (KGA) is extracted from a polar solvent, by contacting the solvent with an extractant (E1) comprising a tertiary amine (I) and a polar organic diluent (II) in a mixing region. 2-Keto-L-gulonic acid (KGA) is extracted from a (preferably aqueous) polar solvent, by contacting the solvent with a first extractant (E1) comprising a tertiary amine of formula NR1R2R3 (I) and a polar organic diluent (II) in a mixing region. R1 - R3 = 6-14C (preferably 8-12C) alkyl. An Independent claim is also included for the production of ascorbic acid (AA), by at least partially lactonizing KGA, extracting KGA from the obtained AA/KGA mixture by the above method and isolating AA from the residual solution.