With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.169447-70-5,(S)-tert-Butyl 2-methylpiperazine-1-carboxylate,as a common compound, the synthetic route is as follows.
tert-Butyl (25)-2-methylpiperazine-1-carboxylate ( 43.1 g, 215 mmol) was added to asolution of aldehyde from Preparation 3 (39.0 g, 195 mmol) in dichloromethane (780mL). The reaction mixture was stirred at room temperature for 10 min then sodiumtriacetoxyborohydride (83.1 g, 391 mmol) was added portion-wise. On complete30 addition the reaction mixture was stirred at room temperature for 4 h. The reaction mixture was carefully quenched with water (200 mL) and extracted withdichloromethane (200 mL). The organic layer was dried over sodium sulphate andconcentrated under reduced pressure. Trituration of the crude product with n-pentane afforded the title compound as an off-white solid. (43.0 g, 57.3%)5 1H NMR (300MHz, DM50-d6) o =7.92 (d, 1=2.2 Hz, lH), 7.68 (d, 1=2.2 Hz, lH), 4.09(m, lH), 3.67 (br d, J= 13.1 Hz, lH), 3.52 (s, 2H), 2.88-3.02 (m, lH), 2.69 (br d,J=ll.l Hz, lH), 2.57 (br d, 1=11.3 Hz, lH), 2.35 (s, 3H), 2.15 (dd, 1=11.3, 3.6 Hz, lH),1.98 (td, 1=11.7, 3.4 Hz, lH), 1.39 (s, 9H), 1.13 (d, J=6.7 Hz, 3H). LCM5 Method 1:10m/z 384.66 [M+H+]; RT = 3.47 min
169447-70-5, As the paragraph descriping shows that 169447-70-5 is playing an increasingly important role.
Reference£º
Patent; LEO PHARMA A/S; JESSIMAN, Alan Stuart; JOHNSON, Patrick Stephen; MAANSSON, Kristoffer; S?RENSEN, Morten Dahl; (156 pag.)WO2018/11201; (2018); A1;,
Piperazine – Wikipedia
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