反应详情

温度

0 °C

BOP (4.43 g, 10 mmol) was poured some more to a solution of 3-oxo-cyclobutanecarboxylic acid (1.14 g, 10 mmol), intermediate 35, 1-(Methanesulphonyl)piperazine (1.64 g, 10 mmol), and triethylamine (4.1 mL, 30 mmol) in DMF (10 mL) in argon under stirring at 0° C. The mixture was stirred for 20 h, evaporated, and the residue was dried at 0.5 mmHg. The residue was subjected to chromatography on SiO2 (200 g, 40-63 μm, CHCl3/hexane 8:2, 9:1, 9.5:0.5→CHCl3→CHCl3/i-PrOH 99:1→95:5) to give the title compound as white crystals in 2.2 g yield. GCMS data: M+ 260 (Calculated for C10H16N2O4S 260.31), 93.5%, r.t. 14.64 min. 1H-NMR data (dmso-d6): 3.56-3.64 (m, 4H), 3.50 (ddd, 1H, J=7.1 Hz, J=9 Hz, J=15 Hz), 3.20-3.29 (m, 4H), 3.08-3.15 (m, 4H), 2.89 (s, 3H).

1. stirringThe mixture was stirred for 20 h
2. customevaporated
3. customthe residue was dried at 0.5 mmHg