反応 #1842300
関連文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07572794B2
反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a stirred solution of 1-(2-hydroxy-ethyl)-piperazine (1.95 g, 15 mmol) in isopropanol (30 mL) at rt was added trimethylsilylisocyanate (2.8 mL, 21 mmol) and the resulting solution stirred overnight before the volatiles were removed in vacuo. The residue was partitioned between CH2Cl2 and water. The aqueous phase was concentrated in vacuo to give 4-(2-hydroxy-ethyl)-piperazine-1-carboxylic acid amide (2.3 g, 88%); 1H-NMR (300 MHz, d6-DMSO) 5.92 (2H, s), 4.40 (1H, t), 3.46-3.52 (2H, m), 3.22-3.34 (4H, m), 2.30-2.39 (6H, m); m/z (ES+) 173 [M+H]+. were removed in vacuo The residue was partitioned between CH2Cl2 and water The aqueous phase was concentrated in vacuo
ソース ID: ord-b5821917fd8e45ed9f93ad4cebeb7dd4