Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 35344-95-7, name is 1H-Pyrazole-4-carbaldehyde, A new synthetic method of this compound is introduced below., Formula: C4H4N2O
A suspension of 1H-pyrazole-4-carbaldehyde (1.00 g, 10.41 mmol) in DCM (30 mL) was stirred under nitrogen. Triethylamine (1.45 mL, 10.41 mmol) was added resulting in a solution. The reaction was cooled to 0 oC with a cooling bath and benzyl carbonochloridate (1.49 mL, 10.41 mmol) was added as dropwise over 5 min maintaining the internal temperature below 10 oC. The reaction was allowed to stir at 4 oC with a cooling bath for 1 h. An aqueous 1M solution of hydrochloric acid (30 mL) was added cautiously. The layers were separated and the aqueous portion was extracted with DCM (2 x 30 mL). The combined organic extracts were washed with water (20 mL) and brine (20 mL). The combined organic extracts were passed through a phase separation cartridge and concentrated under reduced pressure. The resulting yellow residue was purified by flash silica chromatography eluting with a gradient of 0-50percent EtOAc in heptane. Product containing fractions were concentrated under reduced pressure to afford benzyl 4-formylpyrazole-1-carboxylate (1.78 g, 74percent) as a white solid. IR: 1736 (CO), 1674 (CO) cm-1; 1H NMR (400 MHz, CDCl3) 5.51 (s, 2H), 7.35 ? 7.47 (m, 3H), 7.47 ? 7.55 (m, 2H), 8.15 (s, 1H), 8.57 ? 8.71 (m, 1H), 9.96 (s, 1H); 13C NMR (400 MHz, CDCl3) 71.00, 126.11, 128.90, 129.02, 129.35, 133.62, 135.14, 142.86, 148.56, 183.49; HRMS [M+Na]+ measured 253.0578, C12H10O3N2 requires 253.0589.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.