Reference of 22364-25-6,Some common heterocyclic compound, 22364-25-6, name is 4-Bromo-2,3-dimethylaniline, molecular formula is C8H10BrN, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
EXAMPLE 26 Preparation of 2,3-Dimethyl-4-methylthiobromobenzene 603 g (5.85 mol) of tert-butyl nitrite and 375 g of copper powder (5.9 mol) are initially charged in 3000 ml of dimethyl disulfide, and 761 g (3.75 mol) of 4-bromo-2,3-dimethylaniline are added dropwise at from 50 to 58 C. The mixture is subsequently stirred at from 75 to 80 C. for 9 hours. For work-up, the mixture is cooled, the residue is filtered off and the filtrate is washed with saturated aqueous NaHCO3 solution. For purification of the product, the organic phase is separated by distillation. Initially, the excess dimethyl disulfide is separated off at atmospheric pressure. 1870 g of dimethyl disulfide (purity>97% according to GC) are recovered. The residue is subsequently subjected to fractional distillation under reduced pressure (0.1 mbar). Yield: 523 g (60%), purity according to GC 99%.
The synthetic route of 22364-25-6 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; BASF Aktiengesellschaft; US6469176; (2002); B1;,
Bromide – Wikipedia,
bromide – Wiktionary