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. 78703-53-4, name is 1,3-Dimethyl-1H-pyrazole-4-carboxylic acid, A new synthetic method of this compound is introduced below., COA of Formula: C6H8N2O2
To a solution of 10b (578.8 g, 4.13 mol) in DMAC (2.0 L) at 0 C was added thionyl chloride (514.7 g, 4.33 mol) dropwise, maintaining the temperature below 15 C. After addition of DMAC (0.25 L), the mixture was stirred at 0-15 C for 0.5 h. To this mixture was added 8 (500.0 g, 3.93 mol) portionwise, maintaining the temperature below 40 C. After addition of DMAC (0.75 L), the mixture was stirred at 15-40 C for 1 h. Then, H2O (1.0 L), NaOH (346.1 g, 8.65 mol) in H2O (4.5 L), and H2O (3.5 L) were successively added dropwise at 15-40 C. The resulting slurry was stirred for 2 h, and then filtered. Wet solids were washed with H2O (1.5 L) and dried in vacuo at 50 C to give the title compound 13b (923 g, 94%) as a pale brown solid; mp 188-189 C; 1H NMR (500 MHz, DMSO-d6) delta 2.19 (s, 3H), 3.98 (s, 3H), 6.62 (ddd, 4JHF=3.3 Hz, J=8.5, 3.3 Hz, 1H), 6.83 (s, 1H), 7.02 (dd, 4JHF=6.5 Hz, J=3.0 Hz, 1H), 7.07 (dd, 3JHF=10.0 Hz, J=9.0 Hz, 1H), 9.48 (br s, 1H), 9.85 (s, 1H); 13C NMR (125 MHz, DMSO-d6) delta 13.0, 38.5, 107.5, 112.9, 112.9, 115.8 (2JCF=21.3 Hz), 125.0 (2JCF=12.5 Hz), 135.2, 145.4, 149.0 (1JCF=235.0 Hz), 153.3 (3JCF=1.3 Hz), 158.0; IR (ATR) 3229, 1651, 1625, 1547, 1531, 1504, 1452, 1377, 1303, 1274, 1260, 1226, 1178, 1109, 1056, 1024, 973, 893, 850, 817, 804, 788, 771, 746, 678, 638, 624, 595, 527, 510, 461, 451, 432, 422, 412 cm-1; Anal. Calcd for C12H12N3O2F: C, 57.83; H, 4.85; N, 16.86. Found: C, 57.62; H, 4.69; N, 16.88.
The synthetic route of 78703-53-4 has been constantly updated, and we look forward to future research findings.
Reference:
Article; Ishimoto, Kazuhisa; Sawai, Yasuhiro; Fukuda, Naohiro; Nagata, Toshiaki; Ikemoto, Tomomi; Tetrahedron; vol. 69; 40; (2013); p. 8564 – 8571;,
Pyrazole – Wikipedia,
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