Electric Literature of 702-82-9, 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. 702-82-9, name is 3-Aminoadamantan-1-ol. A new synthetic method of this compound is introduced below.
Compound (S)-1-(2-chloroacetyl) pyrrolidine-2-carbonitrile (12.1 g, 70.3mmol) is added to dichloromethane (200mL), stir for 10 minutes, hydroxyl adamantanamine (12.7 g, 66.8mmol) is slowly added to the above solution, the resulting solution is stirred at room temperature for 10 minutes, Potassium carbonate (19. 3g, 140mmol) is added to the reaction solution, the reaction is stirred for 4 hours.The reaction solution has been filtered, the filter cake is washed with dichloromethane (50mL), combined filtrates. Rotate the solvent to get dryness, the residual oil is added to ethyl acetate to dissolve. The resulting ethyl acetate solution is washed with water (50mL X 2), dry over anhydrous sodium sulfate for 2 hours. The desiccant has been removed; and dried then obtained the crude compound 6 (21.2g).Vildagliptin crude (21. 2g) is added into the reactor which is containing 100mL 2-butanone. The mixture is heated to reflux (95 C) and stirred for 30 minutes. The mixture is filtered into a preheated (75 C) reactor; the filter cake is washed with using hot 2-butanone (100mL). The filtrate is heated to reflux for 30 minutes, slowly cool down at room temperature. Let stand overnight. The system is cooled with an ice water bath for 1 hour. The resulting suspension is filtered, the filter cake is washed twice with 2-butanone.The filter cake has been dried, and obtained target product Vildagliptin 12. 4g(white crystal), 61.3%.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,702-82-9, its application will become more common.
Reference:
Patent; Shenzhen Hanyu Pharmaceutical Co., Ltd.; Liu Feimeng; Fang Yihua; Liu Jian; Ma Yaping; Yuan Jiancheng; (10 pag.)CN105884669; (2016); A;,
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