With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.300543-56-0,(R)-1-((4-Chlorophenyl)(phenyl)methyl)piperazine,as a common compound, the synthetic route is as follows.
A mixture containing (4-chlorophenyl)phenyl methylamine free base (4.1 g, 18.8 mmol), N,N-bis(2-chloroethyl)benzyl carbamate (7 g, 26.7 mmol) potassium iodide (1.7 g, 10 mmol) and diisopropyl ethylamine (10 ml) was stirred at 135 C. (oil bath), for 4 hours.While cooling down, 60 ml dichloromethane was added. The mixture was stirred at ambient temperature for 20 min. 35 ml HCl (1M) was added to the dichloromethane. The organic layer was separated, washed with NaCl (10 ml) dried and concentrated to give an oily material (10 g). The impure material was purified with AcOEt/heptane column (3?50%).0.5 grams of above pure material was dissolved in a solution containing 1.3 g NaOH in 1.2 ml H2O and 5 ml 2-propanol. The mixture was heated til 100 C. for 5 h. The mixture was concentrated in vacuo to get rid of 2-propanol and redissolved in 10 ml toluene and 5 ml H2O. The mixture was stirred for 20 min and layers were separated. The organic layer was dried over Na2SO4 and concentrated. To the crude product ethyl acetate (10 ml) was added, followed by addition of 0.2 g oxalic acid dissolved in 1 ml EtOH. The suspension was stirred 4 h at ambient temperature and overnight at 5 C. The solid obtained was filtered off and dried at air to give a solid material (0.3 g, 38.5% yield). 98.86% ee purity.
300543-56-0, 300543-56-0 (R)-1-((4-Chlorophenyl)(phenyl)methyl)piperazine 668697, apiperazines compound, is more and more widely used in various fields.
Reference£º
Patent; Zhu, Jie; US2009/143582; (2009); A1;,
Piperazine – Wikipedia
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