Synthetic Route of 16545-68-9, 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 16545-68-9 as follows.
[000296j Compounds 5-bromo-2-fluoropyridine (25.0 g, 0.12 mol) and cyclopropanol (02, 10.4 g, 0.18 mol) were dissolved in NMP (100 mL) and treated with potassium tertbutoxide (180 mL, lMsolution in THF, 0.18 mol) at 0 C. The solution became dark and cloudy, and warmed. After 30 mm, the reaction mixture was partitioned between ethyl acetate and petroleum ether (500 mL, 1/1 v/v) and water (500 mL). The organic layer was separated, washed with water and 5% aq. LiC1, dried over anhydrous sodium sulfate, filtered and concentrated. The residue was purified with silica gel column chromatography (ethyl acetate in petroleum ether, 10% v/v) to furnish Compound 03. ?H-NMR (CDC13, 400 MHz) major characteristic peaks: (5(ppm) 0.74-0.81 (m, 4H), 4.13-4.18 (m, 1H), 6.88 (d, J= 8.8 Hz, 1H), 7.66 (dd, J 8.8, 2.4 Hz, 1H), 8.26 (d, J 2.4 Hz, 1H).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,16545-68-9, its application will become more common.
Reference:
Patent; BIOMARIN PHARMACEUTICAL INC.; WANG, Bing; WO2015/65937; (2015); A1;,
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