公开(公告)号：DE4226625A1

公开(公告)日：1994-02-17

申请号：DE4226625

申请日：1992-08-12

Applicant: BASF AG

Inventor： KAISER KLAUS DR ,  BALKENHOHL FRIEDHELM DR ,  PAUST JOACHIM DR

IPC: C07F9/655 ,  C07F9/572

Abstract: Process for obtaining the calcium salt of ascorbyl 2-monophosphate from aqueous/alkaline reaction mixtures as they are obtained when ascorbic acid is reacted with a molar excess of phosphorus oxychloride in the presence of a tertiary amine while maintaining a pH of 12 to 13 during the reaction by means of an aqueous alkali metal solution, which process is characterised in that a) starting from a reaction mixture which has been obtained by reacting ascorbic acid with phosphorus oxychloride in the presence of pyridine while maintaining a pH of 12 to 13 by means of an aqueous potassium hydroxide solution, b) the phosphoric acid ions formed during this reaction are precipitated by means of magnesium chloride in amounts of approximately 1 mol per mol of phosphoric acid ions as potassium magnesium phosphate, c) the potassium magnesium phosphate is separated off, d) the pyridine together with some of the water is removed from the remaining aqueous solution by distillation, e) the resulting aqueous solution is reacted with calcium chloride and f) the calcium salt of ascorbyl 2-monophosphate, which crystallises out during this process in the form of the calcium salt, is isolated, or in that, after process step a), the pyridine/water mixture is first removed as described in process step d) and process steps (b), (c), (e) and (f) are subsequently carried out.

公开(公告)号：DE59105210D1

公开(公告)日：1995-05-24

申请号：DE59105210

申请日：1991-01-23

Applicant: BASF AG

Inventor： VON DEESSEN ULRICH DR ,  PAUST JOACHIM DR ,  KAISER KLAUS DR ,  INDEST HELMUT DR

IPC: C07H15/18 ,  C07H15/10 ,  C07H15/26

Abstract: (A) 4-Glycopyranosyloxy-2-methyl -2-buten-1-al derivs. of formula (IVa) and (Va) are new: R4 = CH2OAc or COOMe; Ac = acetyl. (B) Prodn. of retinyl glycosides of formula (I) is effected by (a) reacting an acylated glycoside deriv. of formula (II) with a 4-hydroxy-2-methyl-2 -buten-1-al acetal of formula (III); (b) treating the prod. (IV) with an acid, (c) reacting the resulting aldehdye (V) with a beta-ionylidene -ethyl-triphenyl phosphonium salt of formula (VI) under Wittig conditions; and (d) removing the acyl gps. from the prod.: Z= a linear or branched glycoside gp. comprising 1-20 glycoxide units; Z'=Z in which all OH gps. are replaced by OCOR1; R1 = 1-10C alkyl or aralkyl, R2 and R3 = 1-10C alkyl or 7-10C aralkyl, or R2+R3 = ethylene or propylene opt. substd. by 1-4C alkyl; Y = a leaving gp.; X = a monovalent anion. (C) The use of cpds. (IV) and (V) for prodn. of medicaments is also new.

公开(公告)号：DE4232997A1

公开(公告)日：1994-04-07

申请号：DE4232997

申请日：1992-10-01

Applicant: BASF AG

Inventor： KAISER KLAUS DR ,  PAUST JOACHIM DR

IPC: C07D307/62 ,  C02F1/52 ,  C02F1/58 ,  C07F9/655 ,  C07D307/33 ,  C07F9/09

Abstract: Process for reducing the phosphate content in the effluents from the preparation of salts of ascorbic acid 2-monophosphate, which is characterised in that A. the effluent from the crystallisation of the metal salts of ascorbic acid 2-monophosphate is treated with an alkali metal or alkaline earth metal hypochlorite, chlorine or H2O2 and B. the inorganic phosphate thus obtained by liberation from organically bound phosphorus and/or that still contained in the effluent is precipitated at a pH of 9-12 as sparingly soluble phosphate, in particular as calcium phosphate.

公开(公告)号：DE4137850A1

公开(公告)日：1992-06-04

申请号：DE4137850

申请日：1991-11-16

Applicant: BASF AG

Inventor： ISAK HEINZ DR ,  SCHAEFER BERND DR ,  KAISER KLAUS DR

IPC: C07C69/145 ,  C12P7/62

Abstract: The prepn. of hydroxyalkenyl esters of formula (I) comprises hydrolysing an alkenedioldiacyl deriv. of formula (II) with a base in the presence of pigs liver esterase. In formulae, R1, R2, R3 and R4 are each H, alkyl or aryl; and n and m are 0-5. USE/ADVANTAGE - (I) are intermediates in the synthesis of active ingredients such as herbicides and fungicides, e.g. (I) can be oxidised to formylalkenyl esters which can be reacted with hydroxylamine to give isoxazole derivs. which can be used as precursors for juvenoids. (I) are obtd. in good yields in short reaction times and in high purity. The enzyme is cheap and gives (I) with high selectivity. (II) are readily available.

公开(公告)号：DE59307061D1

公开(公告)日：1997-09-11

申请号：DE59307061

申请日：1993-09-25

Applicant: BASF AG

Inventor： KAISER KLAUS DR ,  PAUST JOACHIM DR

IPC: C07D307/62 ,  C02F1/52 ,  C02F1/58 ,  C07F9/655

Abstract: Process for reducing the phosphate content in the effluents from the preparation of salts of ascorbic acid 2-monophosphate, which is characterised in that A. the effluent from the crystallisation of the metal salts of ascorbic acid 2-monophosphate is treated with an alkali metal or alkaline earth metal hypochlorite, chlorine or H2O2 and B. the inorganic phosphate thus obtained by liberation from organically bound phosphorus and/or that still contained in the effluent is precipitated at a pH of 9-12 as sparingly soluble phosphate, in particular as calcium phosphate.

公开(公告)号：DE4123994A1

公开(公告)日：1993-01-21

申请号：DE4123994

申请日：1991-07-19

Applicant: BASF AG

Inventor： JAEDICKE HAGEN DR ,  KAISER KLAUS DR ,  HAMM MANFRED

IPC: C07C403/06 ,  C07C45/60 ,  C07C67/02 ,  C07C403/00 ,  C07C403/10 ,  C07C403/12 ,  C07C403/14 ,  C07C403/20 ,  C07C403/22 ,  C07D319/06

公开(公告)号：ES2101906T3

公开(公告)日：1997-07-16

申请号：ES93112314

申请日：1993-07-31

Applicant: BASF AG

Inventor： KAISER KLAUS DR ,  BALKENHOHL FRIEDHELM DR ,  PAUST JOACHIM DR

IPC: C07F9/655

Abstract: Process for obtaining the calcium salt of ascorbyl 2-monophosphate from aqueous/alkaline reaction mixtures as they are obtained when ascorbic acid is reacted with a molar excess of phosphorus oxychloride in the presence of a tertiary amine while maintaining a pH of 12 to 13 during the reaction by means of an aqueous alkali metal solution, which process is characterised in that a) starting from a reaction mixture which has been obtained by reacting ascorbic acid with phosphorus oxychloride in the presence of pyridine while maintaining a pH of 12 to 13 by means of an aqueous potassium hydroxide solution, b) the phosphoric acid ions formed during this reaction are precipitated by means of magnesium chloride in amounts of approximately 1 mol per mol of phosphoric acid ions as potassium magnesium phosphate, c) the potassium magnesium phosphate is separated off, d) the pyridine together with some of the water is removed from the remaining aqueous solution by distillation, e) the resulting aqueous solution is reacted with calcium chloride and f) the calcium salt of ascorbyl 2-monophosphate, which crystallises out during this process in the form of the calcium salt, is isolated, or in that, after process step a), the pyridine/water mixture is first removed as described in process step d) and process steps (b), (c), (e) and (f) are subsequently carried out.

公开(公告)号：DE59306642D1

公开(公告)日：1997-07-10

申请号：DE59306642

申请日：1993-07-31

Applicant: BASF AG

Inventor： KAISER KLAUS DR ,  BALKENHOHL FRIEDHELM DR ,  PAUST JOACHIM DR

IPC: C07F9/655

Abstract: Process for obtaining the calcium salt of ascorbyl 2-monophosphate from aqueous/alkaline reaction mixtures as they are obtained when ascorbic acid is reacted with a molar excess of phosphorus oxychloride in the presence of a tertiary amine while maintaining a pH of 12 to 13 during the reaction by means of an aqueous alkali metal solution, which process is characterised in that a) starting from a reaction mixture which has been obtained by reacting ascorbic acid with phosphorus oxychloride in the presence of pyridine while maintaining a pH of 12 to 13 by means of an aqueous potassium hydroxide solution, b) the phosphoric acid ions formed during this reaction are precipitated by means of magnesium chloride in amounts of approximately 1 mol per mol of phosphoric acid ions as potassium magnesium phosphate, c) the potassium magnesium phosphate is separated off, d) the pyridine together with some of the water is removed from the remaining aqueous solution by distillation, e) the resulting aqueous solution is reacted with calcium chloride and f) the calcium salt of ascorbyl 2-monophosphate, which crystallises out during this process in the form of the calcium salt, is isolated, or in that, after process step a), the pyridine/water mixture is first removed as described in process step d) and process steps (b), (c), (e) and (f) are subsequently carried out.

公开(公告)号：DE59201325D1

公开(公告)日：1995-03-16

申请号：DE59201325

申请日：1992-07-08

Applicant: BASF AG

Inventor： JAEDICKE HAGEN DR ,  KAISER KLAUS DR ,  HAMM MANFRED

IPC: C07C403/06 ,  C07C45/60 ,  C07C67/02 ,  C07C403/00 ,  C07C403/10 ,  C07C403/12 ,  C07C403/14 ,  C07C403/20 ,  C07C403/22 ,  C07D319/06

公开(公告)号：DE4003094A1

公开(公告)日：1991-08-08

申请号：DE4003094

申请日：1990-02-02

Applicant: BASF AG

Inventor： DEESSEN ULRICH VON DR ,  PAUST JOACHIM DR ,  KAISER KLAUS DR ,  INDEST HELMUT DR

IPC: C07H15/18 ,  C07H15/10 ,  C07H15/26

Abstract: (A) 4-Glycopyranosyloxy-2-methyl -2-buten-1-al derivs. of formula (IVa) and (Va) are new: R4 = CH2OAc or COOMe; Ac = acetyl. (B) Prodn. of retinyl glycosides of formula (I) is effected by (a) reacting an acylated glycoside deriv. of formula (II) with a 4-hydroxy-2-methyl-2 -buten-1-al acetal of formula (III); (b) treating the prod. (IV) with an acid, (c) reacting the resulting aldehdye (V) with a beta-ionylidene -ethyl-triphenyl phosphonium salt of formula (VI) under Wittig conditions; and (d) removing the acyl gps. from the prod.: Z= a linear or branched glycoside gp. comprising 1-20 glycoxide units; Z'=Z in which all OH gps. are replaced by OCOR1; R1 = 1-10C alkyl or aralkyl, R2 and R3 = 1-10C alkyl or 7-10C aralkyl, or R2+R3 = ethylene or propylene opt. substd. by 1-4C alkyl; Y = a leaving gp.; X = a monovalent anion. (C) The use of cpds. (IV) and (V) for prodn. of medicaments is also new.