Process of production of N-alkyl-2-benzthiazolylsulfeneimides and method of their purification

• Main Authors: KRIZANOVIC KAROL, PINTER JOZEF, SEREDA GABRIEL, VALI KAMIL, STRAUCHOVA ALZBETA
• Format: Patent
• Language: English; Slovak
• Published: 03.05.2007
• Subjects: CHEMISTRY; HETEROCYCLIC COMPOUNDS; METALLURGY; MIXING, e.g. DISSOLVING, EMULSIFYING, DISPERSING; ORGANIC CHEMISTRY; PERFORMING OPERATIONS; PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL; TRANSPORTING

A process of production of N-alkyl-2- benzthiazolylsulfeneimides by means of a reaction of 2-benzthiazolylsulfenyl chloride with an excess of a corresponding alkylamine in an anhydrous reaction medium. Removement of water and moisture from the reaction medium is ensured by azeotropic distillation of a part of the solvent. The method solves also trapping of the excess amine by extraction with water to recycle it in the process, removing of the unconverted raw material from the crude product by chemical refining with aqueous lye and extraction of by-products and pitches by elutriating the product in an organic solvent with the aim to obtain pure benzthiazolylsulpheneimide containing no less than 95 % of the active substance, which can be used as a vulcanization accelerator in ruber mixtures. Spôsob výroby N-alkyl-2-benztiazolylsulfénimidov vzorca (I) reakciou 2-benztiazolylsulfenylchloridus nadbytkom príslušného alkylamínu v bezvodom reakčnom médiu. Odstránenie vody a vlhkosti z reakčného prostredia sa zabezpečuje azeotropickou destiláciou časti rozpúšťadla. Spôsob rieši aj zachytávanie nadbytočného amínu extrakciou vodou na jeho opätovné využitie v procese, odstránenie neskonvertovanej suroviny zo surového produktu chemickou rafináciou vodným roztokom lúhu a extrakciu vedľajších produktov a smôl rozplavením produktu v organickomrozpúšťadle s cieľom získať čistý benztiazolylsulfénimid s obsahom účinnej látky nie nižším ako 95 %, použiteľný ako urýchľovač vulkanizácie v gumárskych zmesiach.