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. 25016-20-0, name is 1-Methyl-1H-pyrazole-3-carboxylic acid, A new synthetic method of this compound is introduced below., HPLC of Formula: C5H6N2O2
The 1-methyl-1 H-pyrazole-3-carboxylic acid R2a (16 mg, 0.127 mmol, 1 .2 equiv) is dissolved in DMF (2 mL), then TEA (59.1 muIota_, 0.442 mmol, 4 equiv) followed by TBTU (39.2 mg, 0.127 mmol, 1.2 equiv). The reaction mixture is stirred for 15 mins, after which the amine hydrochloride Dc is added in DMF (1 mL). The resulting solution is stirred at RT for 16 h. The solution is then filtered through a Millex filter and purified by prep HPLC. (ammonium bicarbonate/MeOH). The pure fractions are combined, concentrated, frozen and lyophilized to provide compound 1016.FIA M.S.(electrospray) : 808.3 (M-H)- , 810.3 (M+H)+ Retention time (min): 5.4 min1H NMR (400 MHz,DMSO-d6): delta 1 .04 (s, 1 H) , 8.76 (s, 1 H), 7.83-7.80 (m, 2H), 7.76 (d, 1 H, J = 2.0Hz), 7.24 (d, 1 H, J = 7.8Hz), 6.59 (d, 1 H, J = 2.3Hz), 6.45 (s, 1 H), 5.70-5.55 (m, 1H), 5.49-5.43 (p, 1H, J= 6.3Hz), 5.43 (s, 1H), 5.2-5.07 (m, 1H), 4.70-4.50 (m,1H), 4.49-4.40 (m, 1H), 4.39-4.25(m, 1H), 4.03-3.85 (m, 1H), 3.95 (s, 3H), 3.89 (s, 3H), 2.95-2.80 (m, 1H), 2.65-2.55 (m, 1H), 2.35-2.19 (m, 2H), 2.0-1.85 (m, 1H), 1.84-1.66 (m, 1H), 1.65-1.5 (m, 3H); 1.49-1.15 (m, 14H); 1.14-0.94 (m, 3H).
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.
Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; LLINAS-BRUNET, Montse; BORDELEAU , Josee; GODBOUT, Cedrickx; LEBLANC, Melissa; MOREAU, Benoit; O’MEARA, Jeffrey; WO2011/63501; (2011); A1;,
Pyrazole – Wikipedia,
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