Synthetic Route of 89-91-8, 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 89-91-8 as follows.
To a solution of lithium aluminium hydride (3.4 g) in tetrahydrofuran (150 mL) was added dropwise a solution of methyl dimethoxyacetate (9.83 mL) in tetrahydrofuran (50 mL) under ice-cooling, and the mixture was stirred at 0 C. for 3 hr. To the reaction mixture was added sodium sulfate decahydrate (45 g) at 0 C., and the mixture was filtered through Celite. The solvent was evaporated under reduced pressure to give the title compound (5.45 g). 1H NMR (300 MHz, DMSO-d6) delta 3.27 (6H, s), 3.32-3.37 (2H, m), 4.29 (1H, t, J=5.5 Hz), 4.69 (1H, t, J=6.1 Hz).
According to the analysis of related databases, 89-91-8, the application of this compound in the production field has become more and more popular.
Reference:
Patent; TAKEDA PHARMACEUTICAL COMPANY LIMITED; KAMEI, Taku; ARIKAWA, Yasuyoshi; OHASHI, Tomohiro; IMAEDA, Toshihiro; FUJIMORI, Ikuo; MIKI, Takashi; YONEMORI, Jinichi; OGURO, Yuya; SUGIMOTO, Takahiro; SETO, Masaki; NISHIDA, Goushi; KAMATA, Makoto; IMOTO, Hiroshi; (132 pag.)US2018/155333; (2018); A1;,
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