In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 75370-65-9 as follows. Safety of 4-Amino-1H-benzo[d]imidazol-2(3H)-one
Amine 2a (1.3 g, 5.9 mmol) was dissolved in 40 ml of AcOEt and at 0C triphosgene (1.75 g, 5.9 mmol) was added to the solution. The mixture was warmed at 80C for 4 hours then evaporated and the residue was dissolved in 5ml of DMF. The solution of the isocyanate was added dropwise to a solution in DMF (10 ml) of compound la (860 mg, 5.77 mmol) and the mixture was warmed at 80C for 8 hours. (TLC AcOEt). The solvent was evaporated and the crude was dissolved in AcOEt (50 ml) and washed with water (1 X 30 ml) and brine. The organic phase was dried over sodium sulfate and concentrated under vacuum. The purification of the crude residue by chromatographic column gave 650mg of a yellow solid. Yield = 28% ‘HNMR (DMSO, 200 MHz) delta 2.51 (6H, bs), 4.43 (2H, d, J = 5.6 Hz), 6.62 (1H, dd, J = 7.6 Hz, J’ = 1 Hz), 6.82 (2H, m), 6.97 (1H, dd, J = 8 Hz, J’ = 1 Hz), 7.32 (1H, s), 7.39 (1H, d), 7.49 (1H, d), 8.35 (1H, bs), 9.99 (1H, bs), 10.59 (1H, bs); [M+1] 394.1 (C18H18F3N5O2 requires 393.36).
According to the analysis of related databases, 75370-65-9, the application of this compound in the production field has become more and more popular.
Reference:
Patent; PHARMESTE S.R.L.; NAPOLETANO, Mauro; TREVISANI, Marcello; PAVANI, Maria Giovanna; FRUTTAROLO, Francesca; WO2011/120604; (2011); A1;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem