4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one, A common heterocyclic compound, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.”80841-78-7
10L autoclave, 520g (0.75mol) Compound 5, DMF3kg, potassium carbonate and 215.3g (1.6mol), stirred at room temperature 1.5-2.5h added to the system after 63.0g (0.38mol) of potassium iodide was added dropwise while – Chloromethyl -5-methyl-1,3-dioxol-2-one 40.0g (0.94mol). Dropping was completed, the reaction at room temperature after 3-4h TLC or HPLC in control, raw reaction was complete. To the system was added ethyl acetate and 3L 3L water and 200g of sodium chloride, stirring separated and the aqueous layer was washed with 3X1L ethyl acetate, the combined organic layers, the organic layer was dried, filtered and the solvent was evaporated cooling is added 0-10 , methanol was added 1600g beating 30min, filtered, then the filter cake was slurried at room temperature in acetonitrile 1600g 30min, filtered to afford intermediate 6 about 553.8g,
The chemical industry reduces the impact on the environment during synthesis, 4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one, , I believe this compound will play a more active role in future production and life.
Reference£º
Patent; Jiangsu Bang Pharmaceutical Co., Ltd.; Zhao, Guangrong; Huan, Shuang; Zhao, Huayang; Liu, Liping; Chen, Guoping; Tang, Jingyu; (19 pag.)CN105481842; (2016); A;,
1,3-Benzodioxole – Wikipedia
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