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公开(公告)号:DE2748905A1
公开(公告)日:1979-05-03
申请号:DE2748905
申请日:1977-11-02
Applicant: BASF AG
IPC: C07C255/24 , C07C121/43 , C07C120/00
Abstract: Prepn. of phenylglycinenitrile-o-carboxylic acid (I) comprises reacting anthranilic acid (II) with HCHO and HCN in an organic solvent at 55-100 degrees (55-70 degrees)C. Pref. the solvent is miscible with water. (I) is an intermediate, by saponification for phenylglycine-o-carboxylic acid which is used in mfr. of indigo. By reacting in a non-aq. solvent the prod. is obtd. free from corrosive by-prods.
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公开(公告)号:DE2638223A1
公开(公告)日:1978-03-09
申请号:DE2638223
申请日:1976-08-25
Applicant: BASF AG
Inventor: TOLKSDORF ERICH DIPL CHEM DR
IPC: C01B21/082 , C01B21/092 , C01B21/10
Abstract: Alkali amides are made by the reaction of molten alkali metals with NH3; and the exhaust gas contg. NH3, from this reaction and/or from any subsequent syntheses in which sodamide is employed, is cleaned, possibly by liquefaction, mixed with further NH3, and recycled for reaction with the alkali metal. The exhaust gas is pref. cleaned via filters before being recycled. The initial raw materials (e.g. sodium) are pref. stored in the absence of air and water to avoid alkali hydroxide impurities, and are melted before being fed into the reactor.
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公开(公告)号:DE2729073A1
公开(公告)日:1979-01-11
申请号:DE2729073
申请日:1977-06-28
Applicant: BASF AG
Inventor: TOLKSDORF ERICH DIPL CHEM DR
Abstract: Prodn. of indigo (I) comprises fusing, at 200-240 degrees C, phenylglycine -o- carboxylic acid salts (II) in a KOH naoh melt having freezing pt. 170-220 degrees C at a pressure of 0.5-10 bar with exclusion of air. The melt is then pured into water and the prod. oxidised. Yields of 90-93% of very pure (I) giving pure colours on cottom (more reddish than that from the Heumannpfleger synthesis.). The use of alkali amides is avoided and the mother liquor left after recovering (I) is suitable for direct processing.
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公开(公告)号:DE2717371A1
公开(公告)日:1978-11-02
申请号:DE2717371
申请日:1977-04-20
Applicant: BASF AG
Inventor: TOLKSDORF ERICH DIPL CHEM DR
IPC: C07C101/16 , C07C101/54
Abstract: Fluid alkyl metal salts of phenylglycine and of phenylglycine-o-carboxylic acid are prepd. by (a) the stepwise saponification of the corresponding nitriles with aq. alkaline waste mother liquors, in the presence of aniline, at between 50 degrees C and b.pt. and (b) evaporation of the reaction mixt. The mother liquors are obtd. from alkali hydroxide/alkali amide melts and contain (by wt. wrt mother liquor) 7-30% NaOH/KOH mixt., 20% Na2CO3/K2CO3 and opt. 10% other components, in addition to smaller quantities of coloured components and organic decompsn. prods. The phenylglycine salt is used as the raw material for indigo prepn. Fluid, mixed phenylglycine salts are obtd. which form less dust in use than Na salts, prepd. by saponifying with NaOH solutions. Use of waste solutions reduces environmental pollution.
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公开(公告)号:DE2729461A1
公开(公告)日:1979-01-04
申请号:DE2729461
申请日:1977-06-30
Applicant: BASF AG
Inventor: TOLKSDORF ERICH DIPL CHEM DR
IPC: C07D215/22 , C07D215/20
Abstract: Prodn. of alkali metal salts (I) of 2,4-dihydroxyquinoline (II) is effected by cyclisation of alkali metal salts (III) of N-acetylanthranilic acid (IV) by adding anhydrous (III) to a NaOH/KOH/NaNH2 melt at 150-175, pref. 168-172 degrees C. The melt is then dissolved in water and cooled so that the mono-Na salt (Ia) crystallises out. Typically, (III) was prepd. by evaporating a paste of (IV) and NaOH soln. to dryness, then added to a NaOH/KOH/NaNH2 melt at 150 degrees C and reacted at 0.8-1.2 bar and max 170 degrees C. The (Ia) yield was 90%, cf. 76% if the temp. was allowed to rise to 180-185 degrees C. Pure (II) was obtd. from the first prod., whereas the second prod. gave discoloured (II) on acidification. (II) is a valuable starting material for the prodn. of pigment dyestuffs. The use of (III) instead of free (IV) leads to the formation of a prod. of better quality, which gives higher yields of (II).
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公开(公告)号:DE2643877A1
公开(公告)日:1978-03-30
申请号:DE2643877
申请日:1976-09-29
Applicant: BASF AG
Inventor: EGER KNUT DIPL ING DR , HOTZ JOHANN DR , TOLKSDORF ERICH DIPL CHEM DR , SCHMIDT HELMUT DIPL CHEM DR , ZETTLER HANS DIETER DIPL ING
IPC: C07D209/34
Abstract: Continuous prepn. of indoxyl-Na, (I), comprises mixing a melt of an alkali metal salt of phenyl glycine with an Na amide/alkali hydroxide melt at 230-250 degrees C in a multiple worm extruder, whereby the melt in mixing- and reaction zone warms up to 260-340 degrees C. After reaction, the melt is discharged. Dwelling times in extruder, after mixing to reaction temp. is 0.5-3 min. The NH3 relased is drawn off in degassing zones. Use of multiple worm extruder allows good mixing of highly viscous melts. Surface of thin layers formed is constantly renewed. Heat released in exothermic reaction is drawn off quickly. No deposits are left in extruder. Process requires a smaller quantity of alkali hydroxide. Yield of (I), indigo quality and indigo yield are not affected.
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