Adding a certain compound to certain chemical reactions, such as: 702-82-9, 3-Aminoadamantan-1-ol, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, 702-82-9, blongs to alcohols-buliding-blocks compound. category: alcohols-buliding-blocks
In the 2L reaction flask, 138.6 g of 3-amino-1-adamantanol was added.105.7g of potassium carbonate,5.3g potassium iodideAnd 900ml acetone,Stir and heat to 50-55C,Intermediate 2 in 110g was added dropwise in 1hMixed with 600 ml acetone,Stirred and incubated for 2 h, TLC detected the reaction was complete.Filter and rinse the filter cake with 300 ml hot acetone.The combined filtrate and washings were concentrated under reduced pressure at 35-45[deg.] C. to a remaining amount of about 770 ml, cooled to 0-10[deg.] C., and incubated for 2 hours while stirring.The filter cake was washed with 100ml of acetone, 40 ~ 50 cake was dried in vacuo 4h, to give a crude vildagliptin 173.5g, a yield of 89.8%. The 3L reaction flask was filled with 170g of crude product and 1870ml of acetone.Stir and heat to 50-55C,Stir until the solids are completely dissolved,Add 8.5g of activated carbon, heat and stir for 0.5h.Heat filtered and washed with 80 ml acetone.The filtrate was stirred and lowered to a temperature of 10-20C.Stir and stir for 2h.After filtration, the filter cake was washed with 80 ml of acetone, and the filter cake was vacuum dried at 40-50 C. for 4 hours to obtain 139.8 g of Vildagliptin with a yield of 82.2%. The content of 3-amino-1-adamantanol was 0.03%. 0.02%, no isomers detected, purity 99.8%.
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; Hebei Medical University; Zhang Kai; Xue Na; Shi Xiaowei; Chen Xinghe; Wang Yabo; Lv Tao; (14 pag.)CN106966947; (2017); A;,
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