Extracurricular laboratory: Synthetic route of 1,3-Dibromoadamantane

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. 876-53-9, name is 1,3-Dibromoadamantane, A new synthetic method of this compound is introduced below., 876-53-9

1. Under nitrogen protection, add 440g of 1,3-dibromoadamantane to a 10L four-necked flask and add 2.0L of Ethyl chloride was stirred well and 500 g of propionic acid aniline was added and stirred well. Add zinc dichloride slowly and stir it well, then heat up to reflux (internal temperature 80-85C). Partially separate the water with a water separator and then use a reflux device. After refluxing at this temperature for 24 hours, the lower layer was a viscous solid and the upper layer was a dichloroethane solvent. Cooled to room temperature, the upper solvent was decanted, 1.0 L DMF was added to warm the solid as a mobile slurry, the slurry was slowly poured into stirred 4.0 L of water, stirred for 30 minutes and filtered to obtain a crude solid wet weight 1015 g, The solid was added to 6L of water for 3.5 hours, filtered and pumped until no liquid was dripped and washed with water (2 x 2L). 1118 g of crude wet weight was obtained, refluxed with 2 volumes of ethanol (3 L) for 1 hour, cooled to room temperature and room The mixture was stirred at room temperature for 1 hour. The wet weight of 439 g was filtered, and used directly for the second-step reaction

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; Shanghai Bodong Chemical Technology Co., Ltd.; Fu Zhiwei; He Baoyuan; Pan Xingang; Yu Wenqing; Li Yongli; Lu Wei; (7 pag.)CN107673977; (2018); A;,
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