Synthetic Route of 1211539-82-0, 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. 1211539-82-0, name is 2,2-Difluorobenzo[d][1,3]dioxol-5-ol. A new synthetic method of this compound is introduced below.
(3) 2.87 g (10.94 mmol) of triphenylphosphine was added to a solution having 1.50 g (7.72 mmol) of ethyl 4-(2-hydroxyethyl)benzoate obtained in the above (1) and 1.38 g (7.95 mmol) of 2,2-difluoro-5-hydroxybenzodioxolane obtained in the above (2) dissolved in 30 ml of THF, followed by stirring for 5 minutes. Then, 4.88 ml (10.73 mmol) of DEAD (2.2 M toluene solution) was added, followed by stirring further for 3 days. The solvent was distilled off under reduced pressure, the obtained crude product was purified by silica gel column chromatography (developing solvent: heptane/ethyl acetate=90/10) to obtain 1.79 g (yield: 66.1%) of ethyl 4-(2-(3,4-(difluoromethylenedioxy)phenoxy)ethyl)benzoate as a pale yellow solid. (0296)H-NMR(300 MHz, CDCl, deltappm): 8.01(d, 2H, J=8.4 Hz), 7.35(d, 2H, J=8.4 Hz), 6.92(dd, 1H, J=8.7 Hz, 2.1 Hz), 6.65(d, 1H, J=2.1 Hz), 6.54(d, 1H, J=8.7 Hz), 4.40-4.30(m, 2H), 4.18-4.05(m, 2H), 3.18-3.08(m, 2H), 1.44-1.30(m, 3H)
At the same time, in my other blogs, there are other synthetic methods of this type of compound,1211539-82-0, 2,2-Difluorobenzo[d][1,3]dioxol-5-ol, and friends who are interested can also refer to it.
Reference:
Patent; ISHIHARA SANGYO KAISHA, LTD.; HIGUCHI, Koji; BOLDBAATAR, DamdinSuren; TAZAWA, Yuta; KANUMA, Michiko; (70 pag.)US2016/192651; (2016); A1;,
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