Continuously updated synthesis method about 28868-76-0

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 28868-76-0, name is Dimethyl 2-chloromalonate, A new synthetic method of this compound is introduced below., Quality Control of Dimethyl 2-chloromalonate

(1) In a 1 L reaction flask equipped with mechanical stirring, temperature display and distillation column, 430 ml of anhydrous dioxane was added.166.6 g of dimethyl chloromalonate and 10 g of dried potassium iodide;(2) 87.5 g of anhydrous potassium fluoride was activated by microwave drying, and added to the above reaction bottle;(3) heating to 100 C under reflux, and reacting for 1 hour;(4) collecting a fraction of 74-78 C through a distillation column;(5) The distillation temperature is up to 78 C to stop heating, to obtain crude dimethyl 2-fluoromalonate;(6) A total of 160g of crude product was collected, and the content of dimethyl 2-fluoromalonate was 91.6%, which was equivalent to 146.6 g of pure product;(7) Refining obtained 136 g of dimethyl 2-fluoromalonate, the content was 99.5%, and the yield was 90.2%.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Sinopharm Group Chemical Reagent Co., Ltd.; Guo Jianguo; Gu Xiaoyan; Wu Xiaolan; Huang Hao; (4 pag.)CN109824512; (2019); A;,
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