SU404346A1 - The method of obtaining, 4-dinitroso-methylaniline - Google Patents

Description

Determination of the whiskers of the method of crushing N, 4-hlHlIlpoeo-Nmethylanil .in, which finds its origin as a modifier of the reaine on the basis of butyl rubber.

A known method for the preparation of S, 4-dinitroso-methylaniline by nitrosation of monomethylaniline from -2 ° to + 12 ° C with sodium nitrite in an environment of glycol saturated with hydrogen chloride. The N-nitrosomethylaniline obtained is rearranged to form 4-nitrosome hydrochloride: ilaniline with do-ba) diethyl ether at 30–40 ° C. 4-1H1 nitro-methyl-1-nitrile nitrate is carried out in aqueous medium and hydrochloride; ° C. Received: S, 4-d. N troso-N-met IL1a1n; IL: I; n separated by filtration, saped and dried.

However, the known method is characterized by the necessity of carrying out the process in the environment of fire and explosive diethyl ether, which is required (this is required (prior to the regeneration of the solvent of the 1Pl1NClIkol), which is required (prior to the use of special steels from the special grades, it is the case of the reference to the target ratio, it is not the case, it is the case, because of the redirection of the ethylene gaLIcol, this is the case, because of the content of ethyleneglycIdIcol), it is required the highest output of the whole great country.

The aim of the invention is to simplify the process and increase the yield of the target product.

For this, the process of re-grouping N-NeT1Rso; methylaniline to 4-nitrosomethylaniline hydrochloride is carried out in hydrochloric acid.

The nitrosation of monomethylaniline is carried out at 1 ~ 10 ° C in an aqueous medium. The obtained N-pitrozometilanilin is separated from the aqueous layer 1, and subjected to a ler group at 25-35 ° C for three hours in hydrochloric acid. The concentration of saline may vary between 30-36%. More concentrated hydrochloric acid is preferred. The 4-nitrosomethylaniline hydrochloride formed as a result of re-precipitation is subjected to a second nitrosis in a cinch (a WATER medium to produce K, 4-dinitroM-methyl aniline A.) The yield of the final product is 80% of the theoretical 3 starting levels. The nitroso compound and the second nitrosation are carried out in two stages, followed by filtration, granulation and drying.

Example. In trezhgorlyuyu

a 250 ml flask equipped with a stirrer, reflux condenser, thermometer was charged with 10.72 g (0.1 g mol) of mymethylaniline, 12 ml of water and 17 ml of hydrochloric acid (specific weight. 1 ,18).

The mixture is well mixed and at 5-10 ° C

Apply iB for 10-15 minutes to 7.25 g (0.105 g mol) of efrita sodium in 12 ml of water. After: d) all the NaNO2 baths continue stirring until the disappearance of mymethylaniline in the reaction mass. Then, the resulting oil MnnIt rozomet1IlaiIl1I1N1a is separated from the IB layer and poured into a 350 ml chopper with a stirrer, a cooler | And a thermometer. iB this box adds 39 ml of 36% to hydrochloric acid (0.45 g mol). The I-1CCio preparation (Nla mass of I-sub | de | ib is IB limit. 25–35 ° C for 3 hours. The resulting suspension is cooled to 10 ° C, diluted with 210 ml of water, and the solution is adjusted to 3 ° C. Then drop by drop, 7.25 g (0.105 g mol) of sodium nitrite in a lead of 40% -iHiOro (Water and ipaiCTBOipa and allow aging for 46 minutes. Suopeneia is filtered, the filter cake is washed with water

And dried at 50 ° C. 13.2 g (80% of the theoretical value) are obtained; M, 4-dinI-prozo-Mmethyl1a-nyl1ina. T. pl. 90-93 ° C.

Subject invention

The method of obtaining H, 4-D1I nit | roso-L-methylanil1IN. A 1 by the way, by hardening N. and mo, but methyl1Nyl; I1H1a, .pe | regrouping: and prepared by NHHHruao. itrozometil, on, and nitriv | oi rovshi last (in iodine environment followed by isolation of the target product by the known icnoco6oiM, differing in that 1, that, in order to simplify the Teliologic process and pov you; -tt litrosomethylalHilin in hydrochloride 4-1nitrozomegilanilIna trade in salt hydrochloride.