SU405896A1 - METHOD FOR PRODUCING SODIUM SALTS OF SUBSTITUTED Z-IMINOTIONAPHTHEN-2-CARBONIC ACID - Google Patents

Description

one

This invention relates to a process for the preparation of sodium salts of substituted 3-, amino-io-io-naphta. N-2-kar | boNoic acid, used as semi-products for the synthesis of thioindigoid, K1 radiators.

Known siozob obtained and sodium salts of the substituted E-1I, m; inot1IOnaphene-2-carbo, but; acid, for example, sodium salts of 6ETOXI-, 6-chloro-4- | methyl- or 6-chloro-3-methylthion -phene-2-, carbonyuic acid, diazotization of the substituted 2-aminophenylthioglycolic acid, aHa, HH | poBaiH, HeM, of the obtained diazo compound, followed by sequential treatment with tetra: sodium sodium sulfide, alkaline .m base P | p and 60 ° C, and simultaneous salting out of the obtained sodium salt salts of the substituted 3-, i.minothio-naphthen-2-carboxylic acid of crystalline sodium chloride To a density of the reaction mass of 1,185-1,200, by filtration, dissolving soda ash in the solution in the presence of activated carbon at 60 ° C and flushing, the sodium salts of schlum (CuS and activated carbon) are emitted by the salt.

The disadvantage of this method is its multistage, the duration of the process and the high consumption of reagents (sodium chloride, calcinated soda, activated carbon).

2

In order to simplify the process technology and improve the quality of the target product, it is proposed to expose the reaction mixture obtained after processing the alkaline | M base to step-by-step crystal of the process: cooling to 2-4 ° C.

Example 1. To 1 liter of a solution containing 31.5 g (0.15 mol) of 2-amino-5 sodium salt .of the kofen.iltiogli.kolevoy to acid (in terms of its lactaim), 18% g of sodium nitrite is cooled to O-2 ° C, the resulting solution slowly pours in. the mixture containing 855 g of water, 61 g of ice and 31 g of salt mislota, and the resulting diazo solution is added to the solution containing 91 ml of water, 17.55 g of pure sodium soda, 5.65 g of copper chloride and 30 g of sodium bicarbonate. Upon termination of the reaction of c, ia.N1Irova.n.i, and into the reaction iMaccy containing co-containing 2-cyano-5-ethoxyphe "lthiogloblum and colonic acid, add a solution of caustic soda to slightly alkaline reakalyi, 9.7 g of sodium tetrasulfide (in terms of polysulfonic sulfur), then the sludge (CuS) is separated, and caustic is added to the filtrate

soda to alkali concentration in the order of 10-15 g / l, heated to 85-95 ° C and kept for 4 hours at this temperature. The reaction: a mass containing a sodium salt of 6-ethoxy-3, notio and naphthen-2-.carboxy acid, stu. Is cooled stepwise, first to 30--32 ° C, and

then to 2-4 ° C. The 6-ethoxn-Zimin salt of the taonaphthene-2-carboxylic acid is filtered off, shrolled with aqueous solutions of sodium chloride (specific weight 1.19-1.2) until no black spot is present on the lead paper. and squeeze.

Examples 2 .and 3. Conducting olytsy analogously to example 1, bottoms of b-chloro-3-methylsyl, and 5-chloro-2-amylophenylthioglyce and acid.

Subject and use of a method for the preparation of the sodium salts of the substituted 3-rm: Pchot. Ionaphene-2-, carbonose acid, diazo-timened.d.m. of the substituted 2-aminophenylthioglycolic acid, cyanoed.} 1m of the obtained diazo compound, with subsequent sequential treatment with tetrasulfide of 1n.r. and alkaline bases upon heating and extraction of the target product by known methods, differing from those) M, which, in order to simplify the process technology and improve the quality of the target product, the reactionary mixture obtained the process of crystallization prn cooled to 2-4 C.