303-26-4 1-((4-Chlorophenyl)(phenyl)methyl)piperazine 9340, apiperazines compound, is more and more widely used in various fields.
With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.303-26-4,1-((4-Chlorophenyl)(phenyl)methyl)piperazine,as a common compound, the synthetic route is as follows.
13.O g (0.2 mol) pulverized zinc are added to the mixture of 300 ml of toluene, 30 ml (0,52 mol) of glacial acetic acid (96% by weight) and 30 ml of methanol with stirring. Subsequently, in three equal portions during 15 minutes, 50.0 g (0.10 mol) (R)-(+)-4-(4-chlorophenyl)-rhohenylmethyl- piperazine- 1 -(2,2,2-trichloroethyl-carbamate) hydrochloride (compound of the Example 6) are added. The temperature of the greyish suspension is raising to approximately 41 to 45 0C in 10 minutes and intense evolution of carbon dioxide occurs.After one hour, the suspension is filtered, the filtrate is mixed with 40 ml of water and 38.5 ml of 25 % by weight ammonium hydroxide solution. The layers are separated, the toluene layer is dried over potassium carbonate and the solvent is evaporated.The thus obtained yellow, oily evaporation residue (approx. 42 g) having the content of 75.5 % calculated as free base, is dissolved in 500 ml of acetone and 12.8 g (0.11 mol) fumaric acid are added. The product, which initially separates in an oily form, is stirred for three hours at the temperature of 25 0C. The crystalline product is filtered and dried until constant weight.Yield, 31.3 g (77.8%) off-white crystals Melting temperature, 146-148 0C. Elemental Analysis {calculated on the basis of the Formula C21Hi3ClN2O4 (402.9)}:Calculated^: 62.61 H: 5.75 Cl: 8.80 N: 6.95 Measured: C: 62.27 H: 5.72 Cl: 8.79 N: 6.84Optical purity (chiral high performance liquid chromatography): 99.S %, 303-26-4
303-26-4 1-((4-Chlorophenyl)(phenyl)methyl)piperazine 9340, apiperazines compound, is more and more widely used in various fields.
Reference£º
Patent; EGIS GYOGYSZERGYAR NYRT.; WO2007/66163; (2007); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics