Analyzing the synthesis route of 5400-75-9

Statistics shows that 5-Methyl-1H-benzo[d]imidazol-2(3H)-one is playing an increasingly important role. we look forward to future research findings about 5400-75-9.

Reference of 5400-75-9, These common heterocyclic compound, 5400-75-9, name is 5-Methyl-1H-benzo[d]imidazol-2(3H)-one, its 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.

5-Methyl-1 ,3-diotahydro-2H-benzimiotadazol-2-one (13.1 g, 88.5 mmol) and phosphorus oxychloride(130 rmL, freshly distillated) was charged into three-neck round-bottom flask. The mixture was heated up to boiling point till homogeneous solution was formed. After that the dried hydrogen chloride was bubbled through inlet gas-pipe into the reaction mixture. The mixture was boiled for 15 hours. Excess of phosphorus oxychloride was distillated in vacuo. Mixture of ice and water (250 ml_) was added to residue. The obtained suspension was cooled to room temperature and filtered. Filtrate was alkalinized by aqueous ammonia solution till pH 8, cooled by cold water and filtered crude 2-chloro-6-methyl-1H- benzimidazole. White powder was crystallized from aqueous methanol (water-methanol: 1.1 , 200 mL), washed by aqueous methanol and dried in desiccator under Phosphorous oxide in vacuo. Yield. 8.17 g (55 percent).

Statistics shows that 5-Methyl-1H-benzo[d]imidazol-2(3H)-one is playing an increasingly important role. we look forward to future research findings about 5400-75-9.

Reference:
Patent; CRYSOPTIX K.K.; WO2009/109782; (2009); A2;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem