Adding a certain compound to certain chemical reactions, such as: 3012-80-4, name is 1-Methyl-1H-benzo[d]imidazole-2-carbaldehyde, belongs to imidazoles-derivatives compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 3012-80-4, COA of Formula: C9H8N2O
100.4 mg of the compound obtained in Synthesis Example 19-2 was dissolved in 1 ml of methanol, and then 1 ml of a 4 mol/l hydrochloric acid/dioxane was added to the solution and the whole was stirred for 3 hours at room temperature. On completion of the reaction, the solvent was distilled off and the residue was then dissolved in methanol, followed by neutralizing with amberlite IRA-410 and distilling the solvent off. The residue was dissolved in 1 ml of anhydrous methanol, and 53.8 mg of 1-methyl-2-formyl benzimidazole was then added to the solution, allowing the reaction thereof for 1.5 hours at room temperature. A reaction solution was concentrated and dried under a reduced pressure, followed by dissolving in 2 ml of methanol again. Subsequently, 25.6 mg of sodium cyanoborohydride was added to the solution and the whole was reacted for 0.5 hour at room temperature. On completion of the reaction, the solvent was concentrated, and the residue was then dissolved in chloroform, followed by washing with distilled water and a saturated salt solution. After the solution was dried with anhydrous sodium sulfate, the solvent was distillated off and the resulting residue was then purified by means of silica gel column chromatography (5 g, chloroform/methanol/water = 7/3/0.5). A 1 mol/l hydrochloric acid was added to the resulting compound, and the mixture was then concentrated and azeotropically co-distilled, and 28.2 mg of hydrochloride of the above-mentioned compound was obtained as a white solid product. MS(FAB,Pos.):m/z=693[M+H]+1H-NMR(500MHz,DMSO-d6):delta=1.87-1.97(4H,m),3.93(3H,s),3.97(3H,s) ,4.46(2H,s),4.55-4.62(1H,m),4.64(2H,s),4.67(2H,s),4.76(2H,d,J =5.6Hz),7.36-7.58(6H,m),7.71-7.79(7H,m),7.93-7.95(1H,m),8.01 (2H,d,J=8.5Hz),8.05-8.08(1H,m),8.73-8.76(2H,m),9.94(2H,brs).
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Reference:
Patent; Kureha Chemical Industry Co., Ltd.; EP1389460; (2004); A1;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem