Synthetic Route of 29671-92-9, These common heterocyclic compound, 29671-92-9, name is Carbamimidic chloride hydrochloride, 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.
2-Amino-6-(4-metho e Experimental procedure taken from Abdillahi et al. [17], Savall ef a/.[18] and Edwards et al. [19]. Ethyl 3-amino-5-(4-methoxyphenyl)thiophene-2-carboxylate (0.832 g, 3.00 mmol) and chloroformamidine hydrochloride (0.517 mg, 4.50 mmol) were mixed with dimethylsulfone (0.847 g, 9.00 mmol) and heated at 140-150 C for one hour. Subsequently, the viscous solution was cooled to room temperature and mixed with an aqueous ice-cooled solution of sodium hydroxide (0.400 g, 10.0 mL). The aqueous solution was extracted with ethyl acetate (3 x 25 mL). The aqueous solution was neutralized with diluted hydrochloric acid (5% v/v) until precipitation started. The precipitates were filtered of and recrystallized from ethanol to yield brown powder (Yield: 36.0%). Mp = 326-328 C. 1H-NMR (DMSO-d6, 400 MHz): 3.81 (s, 3H, CH3), 6.90 (s, 2H, NH2), 7.01 -7.04 (m, 2H, ArH), 7.25 (s, 1 H, ArH), 7.68-7.71 (m, 2H, ArH). 3C-NMR (DMSO-de, 100 MHz): 56.1 (prim. C); 1 4.6 (2C), 1 18.3, 127.4 (2C) (tert. C); 1 10.5, 125.8, 149.7, 155.5, 158.9, 160.1 , 174.4 (quart. C).
Statistics shows that Carbamimidic chloride hydrochloride is playing an increasingly important role. we look forward to future research findings about 29671-92-9.
Reference:
Patent; KTB TUMORFORSCHUNGSGESELLSCHAFT MBH; KUBBUTAT, Michael; SCHAeCHTELE, Christoph; EHLERT, Jan; TOTZKE, Frank; KUNICK, Conrad; WOeLFEL, Sebastian; WEBER, Holger; WO2014/79545; (2014); A1;,
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