Synthetic Route of 756520-66-8, 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. 756520-66-8, name is 1-(2,6-Dichloro-3-fluorophenyl)ethanol. A new synthetic method of this compound is introduced below.
Step 2 (±)3-(1-(2,6,-dichloro-3-fluorophenyl)ethoxy)-2-nitropyridine [00161] To a solution of triphenylphosphine (24.29 g, 92.6 mmol) in THF (dry, 160 ml_) was added DIAD (18.23 ml_, 92.6 mmol) dropwise at 0 C under N2. After addition of DIAD, a solution of 1-(2,6-dichloro-3-fluorophenyl)ethanol (13.35 g, 63.86 mmol) and 3-hydroxy-2-nitropyridine (10.29 g, 73.44 mmol) in THF (anhydrous, 160 ml_) was added dropwise. The ice-bath was removed and the reaction mixture was allowed to warm to room temperature and stirred at room temperature for 4 hrs. The reaction mixture was concentrated by evaporator to give a yellow residue. A saturated solution of NH4CI (200 ml_) was added. The aqueous phase was extracted with EtOAc (3^150 mL). The combined organic phase was washed with brine (2*80 mL), dried over anhydrous Na2S04, concentrated by evaporation in vacuo to give a yellow residue which was purified by CombiFlash (220 g silica gel column, Hexane/EtOAc) to afford (±)-3-(1-(2,6,- dichloro-3-fluorophenyl)ethoxy)-2-nitropyridine (21.1 g, 100%) as a white solid. [00162] 1HNMR (300 MHz, CDCI3): delta 8.04 (d, 1 H), 7.37 (m, 1 H), 7.30 (dd, 1 H), 7.21 (d, 1 H), 7.09 (t, 1 H), 6.10 (q, 1 H), 1.85 (d, 3 H).
At the same time, in my other blogs, there are other synthetic methods of this type of compound,756520-66-8, 1-(2,6-Dichloro-3-fluorophenyl)ethanol, and friends who are interested can also refer to it.
Reference:
Patent; BETA PHARMA CANADA INC.; WANG, Zhaoyin; LI, Lianhai; WANG, Zhigang; WO2013/13308; (2013); A1;,
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