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90-84-6Relevant articles and documents
Electrochemical, Iodine-Mediated α-CH Amination of Ketones by Umpolung of Silyl Enol Ethers
Strehl, Julia,Hilt, Gerhard
supporting information, p. 5968 - 5972 (2020/08/12)
The electrochemical, oxidative Umpolung reaction of silyl enol ethers utilizing simple iodide salts for the synthesis of α-amino ketones is described. The products were isolated in excellent yields of up to 100percent, and various functionalized starting materials were accepted in an undivided electrochemical cell design. Moreover, a sensitivity assessment to ensure an improved reproducibility of the reaction and cyclic voltammetry experiments were performed to postulate a plausible reaction mechanism on their basis.
Enantioselective and Diastereoselective Construction of Chiral Amino Alcohols by Iridium-f-Amphox-Catalyzed Asymmetric Hydrogenation via Dynamic Kinetic Resolution
Wu, Weilong,You, Cai,Yin, Congcong,Liu, Yuanhua,Dong, Xiu-Qin,Zhang, Xumu
supporting information, p. 2548 - 2551 (2017/05/24)
The iridium-f-amphox-catalyzed asymmetric hydrogenation of racemic α-amino β-unfunctionalized ketones proceeds via a DKR (dynamic kinetic resolution) process for the construction of various chiral N,N-disubstituted α-amino β-unfunctionalized alcohols in quantitative yields with excellent enantioselectivities and diastereoselectivities (all products >99% ee and >99:1 dr, TON up to 100 000). Importantly, this catalytic asymmetric hydrogenation with a DKR process provided a highly efficient and powerful synthetic strategy for the preparation of key chiral intermediates of the preclinical antitumor agent (S,S)-R116010.
Synthesis method of amfepramone hydrochloride drug intermediate 2-diethylamino-1-phenylacetone
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Paragraph 0009-0010; 0018-0019, (2017/03/08)
The invention relates to a synthesis method of an amfepramone hydrochloride drug intermediate 2-diethylamino-1-phenylacetone, which comprises the following steps: adding 0.23 mol of alpha-aminophenylacetone into a reaction vessel which is provided with a stirrer, a thermometer, a reflux condenser and a dropping funnel, slowly adding 0.51-0.53 mol of diethylamine, heating the solution to 85-90 DEG C, reacting for 60-90 minutes, lowering the solution to 60-65 DEG C, adding 120ml of toluene, stirring for 60-80 minutes while controlling the stirring rate at 130-150 rpm, filtering, washing the filtrate with an oxalic acid solution, merging the extracting solutions, adding a potassium sulfite solution, regulating the pH value to 8-9, extracting with nitromethane 5-7 times, cooling the solution to 5-9 DEG C, precipitating a crystal, filtering, washing with a salt solution, washing with acetonitrile, and recrystallizing in cyclohexane to obtain the crystal 2-diethylamino-1-phenylacetone.