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    3.
    发明专利
    未知

    公开(公告)号：DE1082907B

    公开(公告)日：1960-06-09

    申请号：DEB0050282

    申请日：1958-09-10

    Applicant: BASF AG

    Inventor： DEUSCHEL DR WERNER

    IPC: C09B48/00

    Abstract: In a process for the production of esters of 2,5-diarylamino - 3,6-dihydroterephthalic acid wherein an ester of succinic acid is treated with an alkali metal alcoholate to give an alkali metal salt of an ester of succinylosuccinic acid, which is acidified to form the free ester and condensed with the appropriate arylamino compound, the first stage of the process is carried out in a solvent comprising a dialkylamide of a carboxylic acid such as dimethylformamide or diethylacetamide, or a N-alkyl lactam such as N-methyl-pyrrolidone, or N-methylpiperidone. The subsequent stages of the process may be carried out in the same solvent as the first stage. The product of the process may be converted into the corresponding 2,5-diarylamino-terephthalic acid by dehydrogenation and saponification. In example 1, a suspension of sodium methylate in N-methyl-pyrrolidone is stirred into diethyl succinate, and the mixture is heated at 110 DEG C. for about 8 hours in an atmosphere of nitrogen. A mixture of aniline and aniline-hydrochloride is then added, and the mixture is maintained at 120 DEG C. for 1 1/2 hours. Water is then added in small portions whereupon crystals of the diethyl ester of 2,5-dianilino-3,6-dihydroterephthalic acid are precipitated. This ester can be converted, without separating it from the pyrrolidone solution, into 2,5-dianilinoterephthalic acid by heating the solution with an aqueous alkaline solution of the sodium salt of meta-nitrobenzenesulphonic acid. The mixture is then diluted with water and acidified in order to precipitate the 2,5-dianilinoterephthalic acid. The following amines may also be condensed with the ester of succinylosuccinic acid:- p-toluidine, o- and p-chloraniline, 2,5-, 2,4, and 3,4-dichloroaniline, p-anisidine, alpha-naphthylamine, and o-, m- and p-aminobenzoic acids. Specifications 742,949 and 751,035 are referred to.

    7.
    发明专利
    未知

    公开(公告)号：DE1149477B

    公开(公告)日：1963-05-30

    申请号：DEB0060672

    申请日：1960-12-29

    Applicant: BASF AG

    Inventor： DEUSCHEL DR WERNER ,  VILSMEIER DR WOLFGANG ,  RIEDEL DR GUENTHER

    IPC: C09B17/00

    Abstract: Fluorubin and fluorubins containing substituents or fused aromatic rings are made by heating to temperatures of about 140 DEG to 400 DEG C. (a) 2: 3-diaminoquinoxaline, (b) a 2: 3-diaminoquinoxaline substituted in the benzene nucleus, (c) a 2: 3-diaminoquinoxaline having fused aromatic rings or (d) a 2: 3-diaminoquinoxaline substituted on an amino group by a 2-aminoquinoxalinyl-(3) radical, if desired in the presence of an organic diluent and an acid catalyst. In processes (b) and (c) unsymmetrical products or mixtures of symmetrical and unsymmetrical products may be obtained. Mixtures of two different 2: 3-diaminoquinoxalines or an unsymmetrical di-(3-amino-2-quinoxalinyl)-amine may be used. In processes (a), (b) and (c) the starting material may be heated first to 100 DEG to 140 DEG C. to convert it to a di - (3 - amino - 2 - quinoxalinyl) - amine and then cyclized by heating to 140 DEG to 400 DEG C. Examples are given.ALSO:In an Example (1) a yellow nitrocellulose lacquer is made by milling together nitrocellulose, dibutyl phthalate, ethyl alcohol, ethyl glycol and a pigment of the formula:- ALSO:A diquinoxalinylamine of the formula a mixture of diquinoxalinylamines of the formulae and diquinoxalinylamines of the formula where R is hydrogen, chlorine, bromine, alkyl or alkoxy are made by heating diaminoquinoxalines of the formulae with compounds of the formulae respectively in N : N-dialkylamides or N-alkyllactams in the presence of alkali at 80 DEG to 200 DEG C. In examples, the following pairs of compounds are heated: (5) 2 : 3-diaminoquinoxaline and 2 - chloro - 3 - amino - quinoxaline; (8) 2 : 3-diamino - 6 - methoxy - quinoxaline and 2-chloro - 3 - amino - quinoxaline and (9) 2 : 3-diamino - 6 - chloro - quinoxaline and 2 - chloro-3 - amino - 6 methyl - quinoxaline. Bis - (2 - aminoquinoxalin - 3 - yl) amine is made (5) by heating 2 : 3-aminoquinoxaline with p-toluenesulphonic acid in N-methylpyrrolidone. 2 : 3-Diaminoquinoxalines are made by heating 2 : 3-dichloroquinoxalines with liquid ammonia at 30 DEG to 130 DEG C. under pressure. In Examples: (1) 2: 3-dichloro-quinoxaline and its 6-methyl derivative, (3) 2 : 3-dichloro-5-methyl-quinoxaline and (4) 2 : 3 : 6-trichloroquinoxaline are heated with ammonia. 2-Amino-3-chloro-quinoxalines are made by treating 2 : 3 - dichloro - quinoxalines with liquid ammonia at -10 DEG to +30 DEG C. under pressure. In an Example, (5) 2 : 3-dichloro-quinoxaline is so treated.

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