10061-02-6, 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 10061-02-6 as follows.
General procedure: Activated Al2O3 (10 g) was stirred with a solution of 0.56 g (5 mmol) of t-BuOK in 10 mL of tert-butyl alcohol under argon for 20 min. The solvent was removed in a vacuum. To the dry residue was added 0.65 g (5 mmol) of ethyl acetoacetate 1b, the mixture was stirred for 1 h under an argon atmosphere. Then, 0.55 g (5 mmol) of (E)-1,3-dichloropropene 2 was added to the mixture, and the mixture was stirred until the reaction completed (8-10 h, GLC monitoring). The solid was washed with ethyl acetate (150 mL) on as hort column, and the solvent was removed in avacuum. The crude product was purified by column chromatography (SiO2, hexane-ethyl acetate, 9 :1?8 : 2). Yield 0.81 g (79%).
According to the analysis of related databases, trans-1,3-Dichloropropene, the application of this compound in the production field has become more and more popular.
Reference:
Letter; Shakhmaev; Sunagatullina, A. Sh.; Alieva; Zorin; Russian Journal of General Chemistry; vol. 87; 10; (2017); p. 2472 – 2476; Zh. Obshch. Khim.; vol. 87; 10; (2017); p. 1723 – 1727,5;,
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