Synthetic Route of 4728-12-5, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 4728-12-5 as follows.
To a suspension of sodium hydride (0.41 g, 10.26 mmol, 60percent in mineral oil) in tetrahydrofuran (15 mL), (2,2-dimethyl-1,3-dioxan-5-yl)methanol (1 , 1 g, 6.84 mmol) was added and the reaction mixture was stirred at room temperature for 10 min. Then methyl iodide (1 .27 mL, 20.52 mmol) was added drop wise at room temperature and the reaction mixture was stirred at room temperature for 6 h. The reaction mixture was quenched with ice water (15 mL) and extracted with ethyl acetate (2 x 30 mL). The combined organic layer was dried over anhydrous sodium sulphate, filtered and concentrated. The crude was purified by silica gel column chromatography using 60percent ethyl acetate in hexane to afford the title compound 5-(methoxymethyl)-2,2-dimethyl-1,3-dioxane (2, 0.65 g, 60percent yield) as a colorless oil. _ NMR (400 MHz, CDCI3) _ (ppm): 3.97-3.93 (m, 2H), 3.76-3.72 (m, 2H), 3.42 (d, J = 6.8 Hz, 2H), 3.34 (s, 3H), 2.00-1 .94 (m, 1H), 1 .42 (s, 3H), 1 .40 (s, 3H).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,4728-12-5, its application will become more common.
Reference:
Patent; CADENT THERAPEUTICS; ANDERSON, David, R.; VOLKMANN, Robert, A.; MENNITI, Frank; FANGER, Christopher; XU, Yuelian; (252 pag.)WO2018/119374; (2018); A1;,
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