Synthetic Route of 4704-94-3, 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 4704-94-3 as follows.
(10a) 1,5,9-trioxaspiro[5.5]undec-3-ylmethanol A mixture of 2-(hydroxymethyl)-1,3-propanediol (3.3 g, 31.1 mmol), tetrahydro-4H-pyran-4-one (3.12 g, 31.2 mmol), p-toluenesulfonic acid monohydrate (268 mg, 1.41 mmol) and benzene (68.3 ml) was refluxed in a round bottom flask equipped with a cooling tube and Dean-Stark for 6 hours. After cooled to room temperature, triethylamine (1 ml) was added to the reaction mixture and the mixture was concentrated. The residue was purified by silica gel column chromatography (silica gel: 200 g, elution solvent: heptane, heptane/ethyl acetate=1/1, 1/3) to obtain the title compound (3.80 g, yield: 64.9%) as a colorless oil. 1H NMR(400 MHz, DMSO-d6) deltappm; 1.67-1.82(5H, m), 3.35-3.42(2H, m), 3.49-3.57(4H, m), 3.65(2H, dd, J=7, 12 Hz), 3.86(2H, dd, J=4, 12 Hz), 4.56(1H, t, J=5 Hz).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,4704-94-3, its application will become more common.
Reference:
Patent; Eisai Co., Ltd.; US2007/10542; (2007); A1;,
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