702-82-9 , The common heterocyclic compound, 702-82-9, name is 3-Aminoadamantan-1-ol, molecular formula is C10H17NO, 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.
In a 2L three-neck flask, 116.3 g (0.6954 moL) of 3-aminoadamantanol was added.70.2 g (0.6954 moL) of triethylamine, 4.8 g (0.02891 moL) of potassium iodide and 650.0 g of acetonitrile,Heat to 75-80C with stirring.100.0 g (0.5793 moL) of (S)-1-(2-chloroacetyl chloride)pyrrolidine-2-carbonitrile (dissolved in 500.0 g of acetonitrile) are added dropwise.2h drop is completed,Stir at 75-80 C for 1 h; TLC test is complete, and the reaction system is cooled to 20-30 C.The filter cake was rinsed with 400 g acetonitrile.Combine the filtrate and remove the solvent under reduced pressure (60C, -0.09–0.1MPa) to obtain an almost white solid.Add 211.0 g of a mixed solvent of ethanol and butanone in a mass ratio of 1:1 and heat to reflux to dissolve.Cool down to 20-30C, stir and crystallize for 1h, continue cooling to -5-5C,The crystals were stirred for 1 h. Filtration, 43g of butanone at 0C, and drying under reduced pressure (60C, -0.09–0.1MPa),127.3 g of white solid powder was obtained (yield 72.4%, HPLC purity 99.10%, Ia content 0.87%),Structural confirmation,
The synthetic route of 702-82-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Yantai Wanrun Pharmaceutical Co., Ltd.; Li Zhong; Hao Yu; Sun Baojia; Lin Peisen; Xiang Longming; Liu Zhigang; (10 pag.)CN104945299; (2017); B;,
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