With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.30459-17-7,1-(4-Trifluoromethylphenyl)piperazine,as a common compound, the synthetic route is as follows.
Acetic acid (33 ??_, 0.59 mmol), HOBt (87 mg, 0.65 mmol), TBTU (208 mg, 0.65 mmol), anhydrous triethylamine (131 ??_, 0.94 mmol) and anhydrous DMF (2 mL) were placed in an oven-dried Schlenk tube under a nitrogen atmosphere. The resulting solution was stirred at room temperature for 15 minutes. A second Schlenk tube was prepared containing 1-(4-(trifluoromethyl)phenyl)piperazine (150 mg, 0.65 mmol) and anhydrous DMF (1 mL) under a nitrogen atmosphere. The resulting solution was stirred until complete dissolution of the piperazine had occurred. The piperazine solution was then transferred, via a cannula, to the first Schlenk tube containing the carboxylic acid. The resulting solution was stirred under nitrogen and monitored by TLC. After 24 hours, the DMF was removed under reduced pressure and the resulting oil was acidified using a 0.1 M HCI solution. The aqueous mixture was extracted with DCM (20 mL, followed by 4 x 10 mL) and the organic layer washed with a saturated sodium bicarbonate solution (3 x 20 mL) and brine (3 x 20 mL). The organic layer was dried over magnesium sulphate and the solvent removed in vacuo. The residue was purified using flash chromatography (4:1 , EtOAc:n-hexane) to obtain the desired product in a 57% yield. H NMR (300 MHz, CDCI3) ? 7.49 (d, J = 8.7 Hz, 2H), 6.91 (d, J = 8.7 Hz, 2H), 3.79-3.76 (m, 2H), 3.65-3.61 (m, 2H), 3.31-3.24 (m, 4H), 2.14 (s, 3H). 3C NMR (75 MHz, CDCI3) 168.0, 151.9, 125.4 (q, J = 3.75 Hz), 1 19.6 (q, J = 33 Hz), 1 18.2 (q, J = 268.5 Hz), 1 15.0, 48.3, 48.0, 45.8, 41.0, 21.3. MS (+ESI) calcd for C13 H15 F3 N2 O m/z: [M + H]+, 273.1209; found 273.1222 [Diff(ppm) = 4.8].
30459-17-7, As the paragraph descriping shows that 30459-17-7 is playing an increasingly important role.
Reference：
Patent; NATIONAL UNIVERSITY OF IRELAND, MAYNOOTH; STEPHENS, John; FINDLAY, John; KINSELLA, Gemma; MARTIN, Darren; DEVINE, Robert; VELASCO-TORRIJOS, Trinidad; WO2013/60860; (2013); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics