反应详情

To a stirred solution of 2-[2-(4-cyclobutyl-piperazin-1-yl)-2-oxo-ethyl]-1,2,3,4-tetrahydro-isoquinoline-6-carboxylic acid (179 mg, 0.5 mmol) and pyrrolidine (71 mg, 1.0 mmol, 2.0 eq.) in DCM (5.0 ml) are added BOP (265 mg, 0.6 mmol, 1.2 eq.) and TEA (101 mg, 1 mmol, 2.0 eq.). The mixture is stirred at rt for 2 hr. Water (5.0 ml) is added to quench the reaction, and the organic layer is collected, dried over sodium sulfate, and concentrated. The residue is purified by PTLC (EtOAc/4% TEA) to give the title compound. 1H NMR (300 MHz, CDCl3) δ 7.23-7.30 (2H, m), 7.01 (1H, d), 3.69 (2H, s), 3.55-3.66 (6H, m), 3.40 (2H, t), 3.35 (2H, s), 2.90 (2H, t), 2.78 (2H, t), 2.66 (1H, m), 2.26 (4H, m), 1.60-2.05 (10H, m); MS (+VE) m/z 411.1 (M++1).

1. customto quench
2. customthe reaction
3. customthe organic layer is collected
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated
6. customThe residue is purified by PTLC (EtOAc/4% TEA)