Reference of 123470-47-3,Some common heterocyclic compound, 123470-47-3, name is 5,6-Difluoro-1H-benzo[d]imidazole-2(3H)-thione, molecular formula is C7H4F2N2S, 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.
Under argon atmosphere, N-[2,4-bis(2,2,2-trifluoroethoxy)-6-methylpyridin-3-yl]-2-[4-[2-(5,6-difluorobenzimidazol-2-ylthio)ethyl]piperazin-1-yl]acetamide (4.0 g, 8.43 mmol), 5,6-difluoro-2-mercaptobenzimidazole (5.8 g, 31.2 mmol) and triphenylphosphine (7.8 g, 29,7 mmol) were dissolved in N,N-dimethylformamide (170 mL), and under cooling with ice diethyl azodicarbonate (40% w/v toluene solution, 11.0 mL, 25.3 mmol) was added dropwise to the mixture, followed by stirring for 1.5 hours at the same temperature. To the reaction mixture, ethylacetate and 1 mol/L of hydrochloric acid, and aqueous layer was separated. The organic layer was further extracted with 1 mol/L hydrochloric acid. The aqueous layer was combined and the resultant mixture was alkalized by sodium hydroxide (1 mol/L), followed by extraction with ethyl acetate. The organic layer was washed with water and saturated brine and then dried over sodium sulfate anhydrate, followed by concentration under reduced pressure. The residue was purified through silica gel column chromatography (developing solvent; chloroform ammonia-saturated methanol=100:3), to thereby yield 2-[4-[2-(5,6-difluorobenzimidazol-2-ylthio)ethyl]piperazin-1-yl]-N-[2,4-bis(2,2,2-trifluoroethoxy)-6-methylpyridin-3-yl]acetamide (4.9 g, yield: 90.1%) as colorless crystals.
The synthetic route of 123470-47-3 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Kowa Co., Ltd.; US2005/20606; (2005); A1;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem