Synthetic Route of 3697-68-5, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 3697-68-5 name is Ethyl 1-(hydroxymethyl)cyclopropanecarboxylate, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
To a solution of ethyl 1-(hydroxymethyl)cyclopropane-1-carboxylate (5.0 g, 34.7 mmol) in dichloromethane (40 mL) and triethylamine (10.5 g, 104 mmol) was added methanesulfonyl chloride (3.66 mL, 47 mmol). The mixture was stirred at 0 C. for 2 h and diluted with dichloromethane (50 mL). The solution was then washed with citric acid (2*40 mL), brine (15 mL), dried over sodium sulfate and concentrated under reduced pressure. The residue was purified by column chromatography (silica gel, 100-200 mesh, 0 to 20% ethyl acetate in petroleum ether) to give ethyl 1-(methylsulfonyloxymethyl)cyclopropanecarboxylate (3.0 g, 39%) as a white solid. 1H NMR (400 MHz, CDCl3) delta 4.34-4.30 (m, 2H), 4.20-4.13 (m, 2H), 3.08 (s, 3H), 1.45-1.41 (m, 2H), 1.29-1.24 (m, 3H), 1.07-1.03 (m, 2H).
At the same time, in my other blogs, there are other synthetic methods of this type of compound, Ethyl 1-(hydroxymethyl)cyclopropanecarboxylate, and friends who are interested can also refer to it.
Reference:
Patent; Genentech, Inc.; Patel, Snahel; Hamilton, Gregory; Stivala, Craig; Chen, Huifen; Daniels, Blake; US2019/127382; (2019); A1;,
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