反应详情

A solution the compound of Example 1 Step 4 (200 mg, 0.55 mmol) in EtOH (25 mL) was treated with N-BOC-1,3-diaminopropane (240 mg, 1.38 mmol) and stirred at reflux for 6 h. The mixture was cooled to room temperature and concentrated under vacuum. The residue was purified by flash chromatography on SiO2 (50% EtOAc/Hexane) to afford the desired product as a yellow oil (165 mg, 66%); 1H NMR (DMSO-d6) δ 7.35 (m, 5H), 5.47 (m, 2H), 4.67 (s, 1H), 2.84 (m, 2H), 2.54 (m, 2H), 2.50 (s, 3H), 1.83 (m, 2H), 1.60 (m, 2H), 1.37 (s, 9H), 0.71 (m, 3H); (LC/MS (ESI): 456 (M+H)+.

1. temperatureat reflux for 6 h
2. concentrationconcentrated under vacuum
3. customThe residue was purified by flash chromatography on SiO2 (50% EtOAc/Hexane)