Electric Literature of 105434-90-0, 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 105434-90-0 as follows.
There was dissolved, in ethanol (3 mL), ethyl 5-amino-1H-pyrazole-3-carboxylate (201 mg, 1.30 mM) and then sodium ethoxide (195 g, 2.86 mM) and diethyl malonate (217 muL, 1.43 mM) were added to the solution. This reaction liquid was stirred for 8 hours, while refluxing the same with heating. This reaction mixture was filtered and then the resulting solid was washed with diethyl ether. After the addition of phosphoryl chloride (10 mL) to the resulting solid with ice-cooling, the resulting suspension was stirred for 3 hours, while refluxing the same with heating. The phosphoryl chloride was distilled off from the reaction liquid, ethanol was then added to the residue with ice-cooling and then the mixture was stirred for 15 minutes. After the concentration of this reaction liquid, the resulting concentrate was purified by the silica gel column chromatography (methanol/methylene chloride=1:100) to thus give the title compound (49.5 mg, overall yield of these two steps: 15%). 1H-NMR (300 MHz, CDCl3): delta 1.45 (t, 3H, J=7.2 Hz), 4.50 (q, 2H, J=7.2 Hz), 7.11 (s, 1H), 7.23 (s, 1H); MS (ESI) m/z 259 (M+H)+.
According to the analysis of related databases, 105434-90-0, the application of this compound in the production field has become more and more popular.