With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.112257-12-2,tert-Butyl 4-(2-bromoacetyl)piperazine-1-carboxylate,as a common compound, the synthetic route is as follows.
4-(2-bromoacetyl)piperazine-1-carboxylate (9.77 mmol, 1 eq.) in methanol (26 ml) at 0C. The reaction vial was sealed and the mixture stirred vigorously overnight at room temperature. The solvent was subsequently evaporated, the residue dissolved in hydrogen chloride (aqueous soln., 0.1 N, 100 ml) and extracted with ethyl acetate (3 x 100 ml). The pH of the recovered aqueous layer was adjusted to 10 by addition of sodium hydroxide (aqueous soln., 1 N), then the organics extracted with ethyl acetate (3 x 100 ml). The combined organic layers were dried over magnesium sulfate, filtered and the solvent evaporated under vacuum to give a light yellow crude product. Further trituration in diethyl ether conducted to the desired amine as a white solid used for the next step without additional purification. C11 H21N3O3; yield 58%; white solid; m.p. 159-160 C; M = 243.30 g/mol; IR (ATR): v = 2974 (w), 1675 (s), 1627 (s), 1417 (m), 1360 (m), 1235 (m), 1172 (m), 1123 (m), 990 (m), 759 (m) cm – ; H NMR (250 MHz, CDCI 3) delta 3.71-3.41 (m, 10H), 1.46 (s, 9H); C NMR (63 MHz, CDCI 3) delta 169.5 (C q), 154.6 (C q), 80.5 (C q), 50.4 (CH 2), 44.6 (2CH 2), 41.7 (2CH 2); HRMS: calcd. for CHH21 3O3 244.1661 , found. 244.1657;, 112257-12-2
The synthetic route of 112257-12-2 has been constantly updated, and we look forward to future research findings.
Reference：
Patent; ASTON UNIVERSITY; GRIFFIN, Martin; RATHBONE, Daniel; BADARAU, Leonas Eduard; WO2014/57266; (2014); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics