摘要 |
PURPOSE: Provided is a method for producing substituted 4,4'-I-amino-stilbene-2,2'-I-sulphonic acid salt in which amine(VI) as an acid interceptor enhances the reaction of sulfo-aniline (IV) and derives of tetrachlorine(III) CONSTITUTION: The production method of the compound of formula (I) comprises: (a) reacting 2 mole-equivs. cyanuric chloride (CNUC) with 1 mole-equiv. of a 4,4'-I-amino-stilbene-2,2'-I-sulphonic acid salt (II) to give (III); reacting (III) with 2 equivs. sulfo-aniline (IV) to give CD. (V); (c) reacting the dichloro CD. (V) with 2 mole-equivs. amine of formula XH,where M=alkali metal ion or opt. substd. ammonium ion; X=N-alkylamino or N,N-I-alkylamino; in the latter case, the two alkyl gps. (opt. cong. in-chain O, N or S) may form part of a satd. 5- or 6-membered heterocycle. Stage (b) is carried out in the presence of amine (VI) as acid-interceptor, by adding sufficient (VI) to maintain a pH of 3.0-7.0, and stage (c) is then carried out by releasing (VI) from its protonated form with the aid of a suitable base. Also claimed is a process for the prodn. of a con. liq. prepn. of CD. (I), in which the crude soln. of (I) is demineralised and cond by means of a membrane process under pressure.
|