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. 25016-12-0, name is 1,3-Dimethyl-1H-pyrazole-4-carbaldehyde, A new synthetic method of this compound is introduced below., Computed Properties of C6H8N2O
In a sealed tube, under N2, 1,3-dimethyl-1H-pyrazole-4-carbaldehyde (284 mg; 2.28mmol) and Ti(iPrO)4 (727 jiL; 3.05 mmol) were added to a solution of intermediate 11(500 mg; 1.52 mmol) in THF (10 mL). The solution was stirred at 50C for 2h. Thereaction mixture was cooled to 5C and iPrMgCl (3.8 mL; 7.61 mmol) was addeddropwise. The reaction mixture was allowed to rise slowly to rt and stirred overnight. The reaction mixture was poured onto a 10% aqueous solution of K2C03 and EtOAc. The insoluble was filtered through a pad of celite then, the organic layer was decanted, dried over MgSO4, filtered and the solvent was evaporated. The residue (866 mg, brownoil) was purified by chromatography over silica gel (Si02 40 g; eluent: from 96% DCM,4% MeOH, 0.4% NH4OH to 93% DCM, 7% MeOH, 0.7% NH4OH). The pure fractionswere collected and the solvent was evaporated to dryness. The residue (496 mg, yellow oil) was recrystallized with diethylether. The precipitate was filtered and dried to give324 mg of compound 161( (45%, white solid).
The synthetic route of 25016-12-0 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; JANSSEN PHARMACEUTICA NV; ANGIBAUD, Patrick, Rene; PANDE, Vineet; HERKERT, Barbara; KROSKY, Daniel, Jason; QUEROLLE, Olivier, Alexis, Georges; PILATTE, Isabelle, Noelle, Constance; PATRICK, Aaron, Nathaniel; (250 pag.)WO2018/50686; (2018); A1;,
Pyrazole – Wikipedia,
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