With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.3405-77-4,5-Methylisoxazole-3-carboxylic acid,as a common compound, the synthetic route is as follows.
2-3 (6.9 g, 54.0 mmol) was dissolved in dry DCM (300 mL) at 0 C.Oxalyl chloride (7.0 mL, 81.0 mmol) was added dropwise. Subsequently, a catalytic equivalent of DMF is added,Stir for 20 minutes, warm to room temperature and stir for 2 h.After the reaction was completed, the solvent was concentrated under reduced pressure and the obtained acid chloride was applied to the next step without purification.Compound 2-2 was dissolved in dry DCM, and the pH of the TEA was adjusted to 7.0 at 0 C, and the acid chloride prepared above was added dropwise.After stirring for 10 minutes, TEA (23.0 mL, 162 mmol) was added dropwise.Raise to room temperature and stir for 2 h. When the reaction is complete, use water, saturated citric acid,The organic phase was washed with saturated NaHCO3 and saturated sodium chloride. The combined organic phases were dried over anhydrous sodium sulfate.The solvent was evaporated under reduced pressure, and the obtained crude product was purified by flash column (PE: EA = 5:1).Compound 2-4 was obtained as a yellow oil (14 g, yield 80%).
The synthetic route of 3405-77-4 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; Nankai University; Shang Luqing; Ma Yuying; He Shuai; Shang Chengyou; (32 pag.)CN110105348; (2019); A;,
Isoxazole – Wikipedia
Isoxazole | C3H3NO – PubChem